Month: December 2020

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. 105486-72-4, name is Ethyl 5-bromo-1-methyl-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of Ethyl 5-bromo-1-methyl-1H-pyrazole-4-carboxylate

4.1.6 1-Methyl-5-(pent-4-en-1-yloxy)-1H-pyrazole-4-carboxylic acid 10b A solution of pent-4-en-1-ol (1.45?mL, 14.0?mmol) in THF (24.0?mL) was cooled to -8?C and treated with 1.0?M sodium hexamethyldisilazane in THF (14.0?mL, 14.0?mmol). The reaction mixture was stirred at the reduced temperature for 5?min before the ice bath was removed. Stirring was continued for an additional 25?min before being treated with a solution of ethyl 5-bromo-1-methyl-1H-pyrazole-4-carboxylate (1.1?g, 4.7?mmol) in THF (24?mL). The reaction mixture was stirred for 1 hour at room temperature before being quenched with 50?mL of sat. NH4Cl. The crude product was extracted with DCM (60?mL x 3), dried with Na2SO4 and concentrated under reduced pressure. This material purified by SiO2 chromatography (ethyl acetate: petroleum ether?=?1:5) to afford 0.65?g impure product 9b mixed with pent-4-en-1-yl 1-methyl-5-(pent-4-en-1-yloxy)-1H-pyrazole-4-carboxylate (produced through transesterification reaction), the mixed esters could both be the raw materials for next hydrolysis, so the mixture was put into next step without further separation. To a solution of the mixed esters in 5?mL MeOH/THF (VMeOH:VTHF?=?1:1) at 0? was added 5?mL 2M NaOH (aq). The mixture was stirred at room temperature for 3?h and MeOH and THF were evaporated in vacuo. The residue was acidified to pH?=?2-3 with 1?N HCl and extracted with ethyl acetate (10?mL?*?3). The combined organic layers were washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure to afford compound 10b as yellow solid (0.45?g, 46%). 1 H NMR (500?MHz, CDCl3) delta 7.84 (s, 1H), 5.89-5.77 (m, 1H), 5.10-5.00 (m, 2H), 4.46 (t, J?=?6.5?Hz, 2H), 3.70 (s, 4H), 2.28-2.19 (m, 2H), 1.93-1.85 (m, 2H); ESI-MS: m/z?=?209 [M-H]-.

According to the analysis of related databases, 105486-72-4, the application of this compound in the production field has become more and more popular.

Related Products of 5334-40-7, The chemical industry reduces the impact on the environment during synthesis 5334-40-7, name is 4-Nitro-1H-pyrazole-3-carboxylic acid, I believe this compound will play a more active role in future production and life.

A stirred solution of S-83 (1.00 g, 6.36 mmol) in THF (10 mL) taken in a round- bottom flask was charged with Et3N (1.3 mL, 9.55 mmol) and DPPA (2.62 g, 9.55 mmol) at room temperature. The reaction mixture was stirred for 6 h at room temperature under nitrogen atmosphere. At this time, t-butanol (10 mL) was added and refluxed for 6 h under nitrogen atmosphere. When TLC showed complete consumption of starting material, the reaction mixture was diluted with the water (10 mL) and extracted with EtOAc (2 ¡Á 10 mL). The combined organic layers were washed with water (10 mL). The organic layers were dried over anhydrous Na2SO4, and concentrated under reduced pressure. The crude product was purified by column chromatography on silica gel using 0? 50percent EtOAc in hexanes as eluent to afford S-91 (0.20 g, 14percent, AMRI lot IN-SKY-C-110) as an off-white solid. The compound was characterized by UPLC analysis. MS-UPLC (MM) m/z 127.2 [M? ]-

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Nitro-1H-pyrazole-3-carboxylic acid, other downstream synthetic routes, hurry up and to see.

Related Products of 3398-16-1, These common heterocyclic compound, 3398-16-1, name is 4-Bromo-3,5-dimethylpyrazole, 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.

PREPARATION 924-Bromo-3,5-dimeth l-1 -(methylthiomethyl)-l H-pyrazoleTo a solution of 4-bromo-3,5-dimethyl-1 H-pyrazole (2.1 Og, 14.3mmol) in acetone (20 ml_) was added K2CO3 (2.37g, 17.1 mmol) followed by chloromethyl methyl sulfide (1.3 ml_, 5.7mmol). The light yellow suspension was stirred at room temperature for 96 hr. At this time the reaction was thick with white precipitate. The reaction mixture was stripped off volatiles, diluted with methylene chloride and filtered. The filtrate was concentrated under reduced pressure to give the title compound as a light yellow oil which was used without further purification.

Statistics shows that 4-Bromo-3,5-dimethylpyrazole is playing an increasingly important role. we look forward to future research findings about 3398-16-1.

Reference of 138786-86-4, These common heterocyclic compound, 138786-86-4, name is Methyl 4-nitro-1H-pyrazole-3-carboxylate, 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.

A mixture of methyl 4-nitro-1H-pyrazole-3-carboxylate obtained in Reference Example 18 (2.0 g, 11.7 mmol), methyl iodide (2.0 g, 14.0 mmol), potassium carbonate (1.62 g, 11.7 mmol) and acetone (60 mL) was stirred at 30C for 5 hr. The mixture was diluted with water, and extracted with chloroform. The extract was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane-ethyl acetate 4:1 – 1:1) to give the title compound, methyl 1-methyl-4-nitro-1-pyrazole-3-carboxylate (Rf value 0.43) (0.95 g, yield 44%) and the title compound, methyl 1-methyl-4-nitro-1H-pyrazole-5-carboxylate (Rf value 0.71) (0.61 g, yield 28%). Methyl 1-methyl-4-nitro-1H-pyrazole-3-carboxylate 1H-NMR (CDCl3):delta 3.99(3H, s), 4.01(3H, s), 8.13(1H, s). Methyl 1-methyl-4-nitro-1H-pyrazole-5-carboxylate 1H-NMR (CDCl3):delta 4.02(3H, s), 4.03(3H, s), 8.01 (1H, s).

Statistics shows that Methyl 4-nitro-1H-pyrazole-3-carboxylate is playing an increasingly important role. we look forward to future research findings about 138786-86-4.

Synthetic Route of 706819-66-1, These common heterocyclic compound, 706819-66-1, name is 2-Bromo-1-(1-methyl-1H-pyrazol-4-yl)ethanone, 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.

General procedure: To a solution of 2-bromo-1-phenylethan-1-one (11a, 5.0 g, 25.12 mmol) and 2-chloropyridin-4-ol (3.9 g, 30.11 mmol) in acetone (75 mL) was added K2CO3 (5.2 g, 37.62 mmol). The reaction mixture was stirred overnight at room temperature. After completion, the mixture was poured into water and extracted with ethyl acetate. The organic layers were combined and then dried with anhydrous sodium sulfate. After removal of the solvent, the residue was purified by a silica gel column chromatography to afford title compound 12a (5.5 g, 88%).

The synthetic route of 706819-66-1 has been constantly updated, and we look forward to future research findings.

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 16034-46-1 as follows. name: 1-Methyl-1H-pyrazole-5-carboxylic acid

To a solution of 1-methyl-1H-pyrazole-5-carboxylic acid (46.6 mg, 0.37 mmol, 1.3 equiv) in DMF (1 ml) were added HATU (140 mg, 0.37 mmol, 1.3 equiv), DIEA (147 mg, 1.14 mmol, 4.0 equiv), and 7-(5-ethyl-1,2,4-oxadiazol-3-yl)-3,4-dihydro-2H-1-benzopyran-4- amine hydrochloride (80 mg, 0.28 mmol, 1.0 equiv). The mixture was stirred overnight and purified by Prep-HPLC with the following conditions: (2-AnalyseHPLC- SHIMADZU(HPLC-10)): Column, XBridge Prep C18 OBD Column, 5 mum,19*150mm; mobile phase, water (10MMOL/L NH4HCO3) and ACN (34.0% ACN up to 47.0% in 8 min); Detector, UV 220nm. This purification resulted in 170 mg (90%) of N-[6-(5-ethyl-1,2,4- oxadiazol-3-yl)-1,2,3,4-tetrahydronaphthalen-1-yl]-1-methyl-1H-pyrazole-4-carboxamide as a white solid. LRMS (ES) m/z 354 (M+H).

According to the analysis of related databases, 16034-46-1, the application of this compound in the production field has become more and more popular.

Synthetic Route of 1280210-79-8,Some common heterocyclic compound, 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, molecular formula is C10H15N3O2, 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.

A vial was charged with (3R,3aR,6R,6aR)-6-[5-(4-bromophenyl)-6-chloro-1-(2-trimethylsilylethoxymethyl)imidazo[4,5-b]pyridin-2-yl]oxy-2,3,3a,5,6,6a-hexahydrofuro[3,2-b]furan-3-ol (501.8 mg, 0.861 mmol), tert-butyl 4,6-dihydro-2H-pyrrolo[3,4-c]pyrazole-5-carboxylate (240.3 mg, 1.148 mmol), tripotassium phosphate (581.6 mg, 2.74 mmol), and copper (I) iodide (37.2 mg, 0.195 mmol). The vial was evacuated (3¡Á) and backfilled with nitrogen. Trans-N,N?-dimethylcyclohexane-1,2-diamine (55 mul, 0.348 mmol) and dioxane (1.7 ml) were added to the vial to give a hazy suspension that was heated to 100 C. for 24 h. The reaction mixture was cooled to room temperature and partitioned between EtOAc (100 ml) and water (100 ml). The aqueous layer was extracted with EtOAc (2¡Á50 ml). The organic layers were combined, washed with brine (1¡Á30 ml), dried over MgSO4, filtered, and evaporated under reduced pressure to give a pale green residue. Flash chromatography of the residue utilizing a 40 g silica RediSep Rf column and employing a 0-100% EtOAc/hexane gradient afforded a mixture of the two pyrazole linked regioisomers as a pale amber foam. LC-MS: calculated for C34H43ClN6O7Si 710.27 observed m/e: 711.29 (M+H)+ (Rt 1.30/2 min)

The synthetic route of 1280210-79-8 has been constantly updated, and we look forward to future research findings.

34605-66-8, name is 3-(2,5-Dimethyl-1H-pyrrol-1-yl)-1-methyl-1H-pyrazole, 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. Computed Properties of C10H13N3

At -78 C, to a solution of 3-(2,5-di methyl- 1 /7-pyrrol- 1 -yl)- 1 -methyl- 1 /7-pyrazolc (step 1 intermediate) (2.0 g, 11.4 mmol) was added n-butyl lithium (1.6 M, 10.55 mL, 16.8 mmol) and the mixture was continued to stir at -78 C for 30 min. The mixture was stirred for 2 h at 0 C and added acetone (1.28 mL, 17.5 mmol) to the solution. The mixture was stirred at RT for 3 h. The mixture was quenched with water and extracted with ethyl acetate. The organic phase was washed with brine and dried over anhydrous sodium sulfate. The solution was filtered, concentrated and the residue obtained was purified by column chromatography to yield 1.0 g of the desired compound. NMR (400 MHz, DMSO-de) d 1.54 (s, 6H), 2.04 (s, 6H), 3.98 (s, 3H), 5.42 (s, 1H), 5.73 (s, 2H), 6.10 (s, 1H).

The synthetic route of 34605-66-8 has been constantly updated, and we look forward to future research findings.

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. 89501-90-6, name is 1-Methyl-1H-pyrazole-3-sulfonyl chloride, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C4H5ClN2O2S

To a 50 mL flask was added 1-methyl-1H-pyrazole-3-sulfonyl chloride (1.12g, 6.22 mmol), ethyl (4aS,6S)-6-[(2,4-dimethoxyphenyl)methylaminoj -1 -(4-fluorophenyl)-5 ,6,7,8-tetrahydro-4H- benzo[flindazole-4a-carboxylate (lila) (1.57g, 3.11 mmol), DCM (8 mL), and triethylamine (1.73 mL, 12.45 mmol) successively. After the reaction was stirred at 40C for 5 h, it was directly concentrated under reduced pressure. The crude product was purified by silica gel column chromatography (Si02, 40%-65% EtOAc/hexanes, gradient elution) to provide ethyl (4aS,6S) -6-[(2,4-dimethoxyphenyl)methyl-( 1- methylpyrazol-3 -yl)sulfonyl-aminoj -1 -(4-fluorophenyl)-5 ,6,7, 8-tetrahydro-4H-benzo [flindazole-4a- carboxylate (ilib) (1.86g, 92% yield) as a yellow solid. m/z(ESI, +ve ion) = 650.3 [M+Hj.

According to the analysis of related databases, 89501-90-6, the application of this compound in the production field has become more and more popular.

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. SDS of cas: 930-36-9

Adding 5.92 g (20 mmol) of FeBr3 to a solution of 8.2 g (100 mmol) of 1-methylpyrazole dissolved in 100 mL of methyl tert-butyl ether at 0 ;Under stirring, 32 g (200 mmol) of Br2 was added dropwise.Stir at room temperature,The end of the reaction was followed by TLC.After confirming the reaction,Filter the system,The filtrate is poured into the water.Use Na2S2O3 solution in sequence,Water washing,Liquid separation.The obtained organic phase was dried over anhydrous magnesium sulfate.The solvent was evaporated under reduced pressure,Got 14.5g(yield: 90.5%, purity 98%)5-bromo-1-methylpyrazole.

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