Month: January 2021

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 83-10-3, name is 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid, A new synthetic method of this compound is introduced below., Safety of 1,5-Dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid

Step 4) 4-(4-(L5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-lH-pyrazole-4-carboxamido)-2,3- difluorophenoxy)picolinamide [0179] To a suspension of 4-(4-amino-2,3-difluorophenoxy)picolinamide (180 mg, 0.68 mmol) and l,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-lH-pyrazole-4-carboxylic acid (161 mg, 0.69 mmol) in DCM (4 mL) was added EDCI (157 mg, 0.82 mmol) and EtaOmicronAlphaTau (19 mg, 0.14 mmol). The mixture was stirred at 45 C for 12 hours, then more 1,5- dimethyl-3-oxo-2-phenyl-2,3-dihydro-lH-pyrazole-4-carboxylic acid (87 mg, 0.37 mmol) was added and the reaction was further stirred at 45 C for 5 hours. The mixture was cooled to rt, quenched with 5 mL of water, and extracted with EtOAc (10 mL x 3). The combined organic phases were washed with brine (10 mL x 3), dried over Na2S04, and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc 100%) to give the title compound as an orange solid (108 mg, 33.2 %). MS (ESI, pos. ion) m/z: 480.1 [M+H]+; *H NMR (400 MHz, DMSO-i): delta (ppm) 11.20 (s, 1H), 8.55 (d, J= 5.7 Hz, 1H), 8.34 (m, 1H), 8.16 (br s, 1H), 7.76 (br s, 1H), 7.64 (m, 3H), 7.59 (d, J= 7.8 Hz, 1H), 7.46 (m, 3H), 7.28 (m, 1H), 3.38 (s, 3H), 2.71 (s, 3H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference of 25016-11-9, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 25016-11-9, name is 1-Methyl-1H-pyrazole-4-carbaldehyde belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below.

Step 1 : methyl 14-cvclohexyl-6-f(l -methyl- 1 H-pyrazol-4-yl )methyl]-5.6.7, 8-tetrahvdroindolo[2, 1 – a] [2,5 Jbenzodiazocine-] 1 -carboxylate; To a solution of methyl 14-cyclohexyl-5,6,7,8-tetrahydroindolo[2,l-a][2,5]-benzodiazocine-l l- carboxylate (prepared as described in Example 48, Step 3) in MeOH (0.06 M), 1 -methyl- lH-pyrazole-4- carbaldehyde (3 eq) was added and the pH adjusted to pH 4 with acetic acid. The solution was stirred at RT for 30 mins before addition of NaBH3CN (1.5 eq). The reaction was stirred at RT for 16 h. The reaction was quenched with saturated aqueous NaHCO3 and extracted with EtOAc (x2). The combined organics were washed with brine, dried (Na2SO1O, filtered and concentrated in vacuo to give the title compound as a viscous oil (quantitative); MS (ES+) m/z 483 (M+H)+

The synthetic route of 1-Methyl-1H-pyrazole-4-carbaldehyde has been constantly updated, and we look forward to future research findings.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 25016-20-0, name is 1-Methyl-1H-pyrazole-3-carboxylic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 25016-20-0

Acid R2b (8.2 mg, 0.065 mmol, 1.3 equiv) is dissolved in DMF (0.5 mL), then TEA (35 muIota_, 0.25 mmol, 5.0 equiv) is added followed by TBTU (19 mg, 0.060 mmol, 1.2 equiv). The solution is stirred for 15 mins, after which the amine hydrochloride Da (37 mg, 0.050 mmol) is added in DMF (0.5 mL). The solution is stirred at RT for 16 h. Water (2 mL) is added and the organic layer is extracted with EtOAc (3 x5 mL). The solvent is then evaporated and purified on prep HPLC (MeCN:H20, 0.1% TFA). The pure fractions are combined, concentrated, frozen and lyophilized to provide compound 1003. FIA M.S.(electrospray): 806.4 (M+H)+ Retention time (min) = 5.5 min1H NMR (400 MHz,DMSO-d6): delta 11.03 (s, 1H) , 8.81 (s, 1H), 7.83 (d, 1H, J = 8.8 Hz), 7.78-7.74 (m, 2H), 7.08 (d, 1H, J = 9.3 Hz), 6.60 (d, 1H, J = 2.3 Hz), 6.37 (s, 1H), 5.67-5.58 (m, 1H), 5.53-5.42 (m, 2H), 5.14 (dd, 1H, J = 9.5, 9.2 Hz), 4.64-4.57 (m, 1H), 4.51 (d, 1H, J= 11.6 Hz), 4.38 (dd, 1H, J= 9.4, 7.0 Hz), 4.01 (dd, 1H, J = 11.8, 3.5 Hz), 3.89 (s, 3H), 3.88 (s, 3H), 2.96-2.88 (m, 1H), 2.65-2.57 (m, 1H), 2.44 (s, 3H), 2.40-2.28 (m, 2H), 2.00-1.89 (m, 1H), 1.88-1.77 (m, 1H), 1.62-1.51 (m, 3H), 1.50-1.33 (m, 11H), 1.31-1.19 (m, 2H), 1.14-0.98 (m, 4H).

The synthetic route of 25016-20-0 has been constantly updated, and we look forward to future research findings.

Related Products of 930-36-9, These common heterocyclic compound, 930-36-9, name is 1-Methylpyrazole, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Example 1. Synthesis of 2-Methyl-2H-pyrazole-3-carbaldehyde In a dry 50 ml Vial is placed a solution of 1.642 g (20 mmol) N-Methylpyrazole in 30 ml dry THF. The mixture is cooled to -20C and while stirring 8 ml (20 mmol, 2.5M in hexane) n-BuLi-solution is slowly added. The reaction mixture is stirred for 2.5 h at -20 C. With vigorous stirring 4.7 ml (4.39g, 60 mmol) dry DMF is slowly added at -20 C and the mixture kept at this temperature for 1h. The reaction mixture is then poured into 100 ml of a 1M acetic acid / sodium acetate buffer (pH: 4.5), 50 ml MTBE is added and the organic layer is separated, washed with 50 ml sat. Na2CO3-Solution to remove excess acetic acid (extraction with ethyl acetate leads to DMF in the final product). The organic layer is separated, dried with MgSO4 and the solvent is removed by om a rotary evaporator. The crude product is purified by vacuum distillation (bp: 67 C, 21 mbar). 3 preparations which were distilled together yielded 5.969g (54 mmol, 90%) of the title compound. 1H-NMR (300 MHz, CDCl3): 4.18 (s, 3H, CH3-N), 6.91 (d, 1H, 3J=2.0 Hz, CH=C-N), 7.53 (d, 1H, 3J=2.0 Hz, CH=N), 9.87 (s, 1H, CH=O) ppm. 13C-NMR (100 MHz, CDCl3): 39.31 (CH3-N), 114.78 (CH=C-N), 138.54 (CH=N), 138.98 (CH=C-N), 179.83 (CH=O) ppm.

Statistics shows that 1-Methylpyrazole is playing an increasingly important role. we look forward to future research findings about 930-36-9.

Synthetic Route of 1145-01-3,Some common heterocyclic compound, 1145-01-3, name is 3,5-Diphenyl-1H-pyrazole, molecular formula is C15H12N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

2d. Under argon atmosphere, CuI (0.38 g, 2 mmol), proline(0.46 g, 4 mmol) and K2CO3(2.76 g, 20 mmol) were added toa dimethyl sulfoxide (15 mL) solution of 6-bromopyridine-2-carboxylate (4.60 g, 20 mmol) and 3,5-diphenylprazole (4.44 g,20 mmol). The formed mixture was stirred at 80C overnight.Water was added after cooling down to room temperature, and theresulting mixture was extracted with ethyl acetate (3¡Á 20 mL). Theorganic layers were combined and the solvent was removed to givethe crude product, which was purified by column chromatography(3.76 g, 83% yield).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3,5-Diphenyl-1H-pyrazole, its application will become more common.

35691-93-1, name is Ethyl 3,5-dimethyl-1H-pyrazole-4-carboxylate, belongs to pyrazoles-derivatives compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. SDS of cas: 35691-93-1

4.2.1 Ethyl 2,5-dimethylpyrazolo[1,5-a]quinoline-3-carboxylate (5a) Condition A: A mixture of 2-fluoroacetophenone 3a (138 mg, 1.00 mmol), 1H-pyrazole 2a (202 mg, 1.20 mmol) and K2CO3 (420 mg, 3.00 mmol) in DMF (5.0 mL) was stirred at 120 C for 16 h. After monitoring the end of the reaction on TLC, the mixture was cooled to room temperature and diluted with water. The resulting mixture was extracted with ethyl acetate twice. The combined organic layers were washed with water twice, dried over MgSO4 and the solvent was removed in vacuo to afford a residue. The residue was purified by flash column chromatography (hexane:EtOAc=5:1) on silica gel to afford 5a (92.0 mg, 34% yield). Condition B: The reaction was carried out with Cs2CO3 instead of K2CO3 under the same conditions as that of Condition A to afford 5a (210 mg, 78% yield).

The synthetic route of 35691-93-1 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 1192-21-8, name is 1-Methyl-1H-pyrazol-5-amine, molecular formula is C4H7N3, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Formula: C4H7N3

1-Methyl-1H-pyrazol-5-amine (4.85 g, 49.9 mmol) and diethylethoxymethylenemalonate (10 mL, 50 mmol) were heated at110 C for 1.5 h. The ethanol by-product was removed by evaporationunder reduced pressure. Phosphoryl trichloride (12.1 mL,130 mmol) was added and the mixture was heated at 110 C for3.5 h. The mixture was cooled to room temperature and MeCN(5 mL) was added, and then the solution was further cooled downto 10 C. Water (80 mL) was added slowly maintaining the temperaturebelow 10 C and the suspension was stirred at ambient temperatureovernight. The resultant solid was collected by filtration,washed with minimum amount of water and dried under reducedpressure to afford the title compound (6.7 g, 54percent) as a white solid;1H NMR (400 MHz, DMSO-d6) d = 8.96 (s, 1H), 8.40 (s, 1H), 4.38 (q,J = 7.0 Hz, 2H), 4.10 (s, 3H), 1.36 (t, J = 7.0 Hz, 3H); 13C NMR(101 MHz, DMSO-d6) d = 163.6, 151.0, 150.7, 137.8, 132.2, 118.0,115.1, 61.5, 34.2, 14.0. LCMS (Method A, UV, ES): RT = 1.00 min,[M+H]+ = 240, 242, 97percent purity. These data were in agreement withthose reported in the literature.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1192-21-8, its application will become more common.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 288148-34-5, name is 1-Methyl-1H-pyrazole-4-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 288148-34-5

General procedure: 1mL of a solution containing arylsulfonyl chloride or arylacyl chloride or arylisocyanates ([Diversity reagent 13{1-8},13{9-10} or 13{11-12}, 0.40 mmol, 5 equiv) in CH2Cl2was added to the resin followed by addition of DIEA (0.88 mmol, 11 eq). Thereactors were shaken for 2 h at room temperature. The resin was drained andwashed with DMF (3 x 5 mL), MeOH (1 x 5 mL), and CH2Cl2(3 x 5 mL), and dried under low vacuum. The procedure described abovewas repeated.

According to the analysis of related databases, 288148-34-5, the application of this compound in the production field has become more and more popular.

Application of 37622-90-5,Some common heterocyclic compound, 37622-90-5, name is Ethyl 4-pyrazolecarboxylate, molecular formula is C6H8N2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The solution of ethyl 1H-pyrazole-4-carboxylate (2.5 g, 17.9 mmol), and iodomethane (3.1 g, 21.5 mmol) in DIVIF (10 mL) was added K2C03 (5.0 g, 35.8 mmol) and then the reaction mixture was stirred at room temperature for 16 hrs. Water (50 mL) was added to the mixture and then extracted by EA (50 mL x2). The organic layer was washed with brine (40 mL), dried over Na2SO4, and concentrated under reduced pressure. The residue was purified by silica gel column (PE/EA = 8/1) to give the ethyl 1-methyl-1H-pyrazole-4-carboxylate (214 mg, yield: 85%) as a colorless oil. ?H NIVIR (300 IVIHz, DMSO-d6): oe = 8.28 (s, 1H), 7.82 (s, 1H), 4.26 (q, J= 6.9 Hz, 2H), 3.87 (s, 3H), 1.25 (t, J= 6.9 Hz, 3H). MS: m/z 155.3 (M+H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Ethyl 4-pyrazolecarboxylate, its application will become more common.

In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 345637-71-0, name is 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid belongs to pyrazoles-derivatives compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 2-(5-Methyl-3-(trifluoromethyl)-1H-pyrazol-1-yl)acetic acid

Example 1 : This example illustrates the preparation of 3-chloro-2-hydroxy-N-(3-{1-[2-(5- methyl-3-trifluoromethyl-pyrazol-1-yl)-acetyl]-piperidin-4-yl}-phenyl)-benzamide (Compound No. I. U.003) a) Preparation of 1-[4-(3-amino-phenyl)-piperidin-1-y l]-2-(5-methyl-3-trifluoromethyl- pyrazol-1 -yl)-ethanoneTo a solution of (5-methyl-3-trifluoromethyl-pyrazol-1-yl)-acetic acid (0.49 g, 2.35 mmol) in DMF (10 ml_) is added triethylamine (0.65 ml_, 4.7 mmol), followed by 1-hydroxy-7- benzotriazole (0.32 g, 2.35 mmol) and 1-Ethyl-3-(3-dimethyllaminopropyl)carbodiimide hydrochloride (0.45 g, 2.35 mmol). After stirring 15 min at RT, 3-Piperidin-4-yl-phenylamine hydrochloride (0.50 g, 2.35 mmol) is added to the reaction mixture. After stirring overnight at RT, solvent is evaporated and the resulting yellow oil is dissolved in ethylacetate (20 ml_), washed with saturated aqueous sodium bicarbonate solution (20 ml_), and brine (20 ml_). The organic layer is dried over sodium sulfate, filtered, and evaporated under reduced pressure to give 1-[4-(3-amino-phenyl)-piperidin-1-y l]-2-(5-methyl-3-trifluoromethyl-py razol- 1-yl)-ethanone as a crude mixture of good enough purity for the next step (0.86 g, quantitative). 1 H-NMR (400 MHz, MeOD): delta =1.52-1.63 (m, 1 H), 1.64-1.73 (m, 1 H), 1.80-1.93 (m, 2H), 2.33 (s, 3H), 2.68-2.81 (m, 2H), 2.99 (s, 2H), 3.21-3.27 (m, 1 H), 4.02-4.09 (m, 1 H), 4.55-4.62 (m, 1 H), 5.12-5.28 (q, 2H), 6.41 (s, 1 H), 6.55-6.60 (m, 1 H), 6.61-6.62 (m, 1 H), 7.00-7.07 (t, 1 H), 7.99 (s, 1 H). MS: m/z = 367 (M+1).

The synthetic route of 345637-71-0 has been constantly updated, and we look forward to future research findings.