Day: February 8, 2021

Adding a certain compound to certain chemical reactions, such as: 398495-65-3, name is 5-tert-Butyl 1-ethyl 3-aminopyrrolo[3,4-c]pyrazole-1,5(4H,6H)-dicarboxylate, belongs to pyrazoles-derivatives compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 398495-65-3, HPLC of Formula: C13H20N4O4

EXAMPLE 28 Preparation of 3-(2-Naphthalen-2-yl-propionylamino)-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester To a solution of 2-naphthalen-2-yl-propionic acid (1.48 g. 7.4 mmol) in DCM (40 ml) and DMF cat., (COCl)2 (0.83 ml, 9.65 mmol) in DCM (10 ml) was added dropwise. The mixture was stirred at r.t. for 30 min. The reaction mixture was concentrated under vacuum, reconstituted twice with toluene and concentrated. A solution of the obtained acyl-chloride in THF (40 ml) was added slowly to a mixture of 3-amino-4,6-dihydro-pyrrolo[3,4-c]pyrazole-1,5-dicarboxylic acid 5-tert-butyl ester 1-ethyl ester (2.0 g, 6.75 mmol) and DIEA (5.8 ml, 33.3 mmol) in THF (40 ml) at 0-5 C. The reaction was allowed to reach r.t. and stirred overnight. The mixture was filtered and the solution evaporated to dryness under vacuum. The resulting residue was dissolved in DCM and the obtained solution was washed with brine, dried over sodium sulfate, filtered and evaporated to dryness. The crude product was purified by flash-chromatography (eluent:ethyl acetate/cyclohexane 3/7 then 4/6) to give 3.0 g (93% yield) of the title compound as a white solid.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 5-tert-Butyl 1-ethyl 3-aminopyrrolo[3,4-c]pyrazole-1,5(4H,6H)-dicarboxylate, and friends who are interested can also refer to it.

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. 27258-33-9, name is 1-Methyl-1H-pyrazole-5-carbaldehyde, A new synthetic method of this compound is introduced below., name: 1-Methyl-1H-pyrazole-5-carbaldehyde

B); With ligand (S)-2-piperidinyl-1,1,2-triphenylethanol and diethylzinc at -10 C In a 20 ml vial 50 mg (0.21 mmol) 2-aminoethyl-dithienyl-borinate and 9.3 mg (0.025mmol) of ligand (S)-2-piperidinyl-1,1,2-triphenylethanol (10 mol%) is placed. The vial is closed and flushed with argon. Dry toluene (2 mL) is added and the vial is placed in a cooling bath of -10 C. Diethylzinc (0.7 mL, 0.7 mmol, 2M solution in toluene) and 25 mul (0.25 mmol) 2-methyl-2H-pyrazole-3-carbaldehyde is added and the reaction mixture is stirred for at least 12 h at -10 C. Work-up is conducted as described in Example 2a affording the title compound (24 mg, 51%) in 70% ee.

The synthetic route of 27258-33-9 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 139756-02-8, name is 4-Amino-1-methyl-3-N-propyl-1H-pyrazole-5-carboxamide, molecular formula is C8H14N4O, 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. category: pyrazoles-derivatives

Preparation of 4-[2-Propoxy Benzamido]-1-Methyl-3-Propyl-5-Carbamoyl Pyrazole To a solution of 25 g of 2-propoxy benzoic acid dissolved in dichloromethane, 66 g of thionyl chloride was added and stirred for 3 hours under reflux. After reaction was completed, the solvent and excessive thionyl chloride were distilled off under reduced pressure. To the residue was added 200 ml of dichloromethane (reaction solution 1). In another container, to 24 g of 1-methyl-3-propyl-4-amino-5-carbamoyl pyrazole in dichloromethane was added 13.4 g of triethylamine and 100 mg of dimethylaminopyridine and then cooled to 0 C., to which said reaction solution 1 was slowly added while maintaining the temperature of the solution at 0 C., and then stirred for 1 hour. The reaction mixture was successively washed with water, saturated aqueous sodium bicarbonate solution and brine. The organic layer was dried over anhydrous sodium sulfate and then filtered. The filtrate was concentrated under reduced pressure to obtain a crude product and then triturated with hexane to give 39 g of the title compound. 1H NMR (CDCl3): 0.91(t,3H), 1.05(t,3H), 1.62(m,2H), 1.89(m,2H), 2.52(t,2H), 4.06(s,3H), 4.18(t,2H), 5.57(br s,1H), 7.09(m,2H), 7.52(m,1H), 7.73(br s,1H), 8.26(dd,1H), 9.45(br s,1H)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 139756-02-8, its application will become more common.

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. 852227-86-2, name is 5-(Chloromethyl)-1,3-dimethyl-1H-pyrazole, A new synthetic method of this compound is introduced below., Computed Properties of C6H9ClN2

A solution of 7d (58 mg, 0.20 mmol, 1.0 equiv) in anhydrous DMF (0.8 mL) was treated with 60% sodium hydride (18 mg, 0.44 mmol, 2.2 equiv). After stirring at room temperature for 5 min, 5-(chloromethyl)-l,3-dimethyl-lH-pyrazole (63 mg, 0.42 mmol, 2.1 equiv) was introduced. Then the mixture was stirred at room temperature for 2 hours. The reaction was quenched with saturated aqueous NaHCO3. The resulting solution was extracted with ethyl acetate. The combined extracts were washed once with brine, dried over Na2SO4, filtered and concentrated in vacuo. The residue was purified by prep-TLC (ethyl acetate/dichloromethane/ methanol 10/10/1, 2 runs) to afford compound 30 (50 mg, 50%) as a white solid. MS 505 (MH)+, 503 (M-H)”. Purity 99% (HPLC).

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.

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. 1254717-53-7, name is (5-(Trifluoromethyl)-1H-pyrazol-3-yl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: (5-(Trifluoromethyl)-1H-pyrazol-3-yl)methanamine

Step i: (3-(Trifluoromethyl)-1H-pyrazol-5-yl)methanamine (0.7 g, 4.2 mmol, 1 eq) was charged in dichloromethane (70 ml) at room temperature, then to that TEA (0.42 g, 4.2 mmol, 1 eq) was added at room temperature and stirred for 10 min and cooled to 0-5 C. (Boc)2O (0.92 g, 4.2 mmol, 1 eq) was added drop wise to reaction mixture for 30 min and maintained for 3 h at 0-5 C. Progress of the reaction was monitored by the TLC (30% Ethyl acetate/Hexane). On completion of the reaction, dichloromethane was distilled, the residue obtained was treated water (50 ml) and extracted with ethyl acetate (100 ml). The combined organic layer was dried over sodium sulphate, distilled the solvent under vacuum. The obtained crude was purified with column chromatography to yield the required product as a white colored solid (0.5 g, 44% yield).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1254717-53-7.

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. 1260243-04-6, name is Ethyl 5-amino-1H-pyrazole-4-carboxylate, A new synthetic method of this compound is introduced below., COA of Formula: C6H9N3O2

To a solution of ethyl 5-amino-lH-pyrazole-4-carboxylate (1.0 g, 6.45 mmol) in n- BuOH (1 ml) was added to ethyl 3-(2H-l,3-benzodioxol-5-yl)-3-oxopropanoate (1.83 g, 7.75 mmol and TsOH (55 mg, 0.32 mmol), and the reaction mixture was stirred for 20 h at 130C. The solid was collected by filtration and washed with methanol (3 x 10 ml) and dried in an oven under reduced pressure to afford ethyl 5- (2H-l,3-benzodioxol-5-yl)-7-oxo-4H,7H-pyrazolo[l,5-a]pyrimidine-3-carboxylate as a yellow solid (1.8 g, 85 ). LC/MS (ES, m/z): [M+H]+ 328.0 *H NMR (300 MHz, DMSO) delta 11.52 (s, 1H), 8.25 (s, 1H), 7.39 (d, /= 1.8 Hz, 1H), 7.31 – 7.35 (m, 1H), 7.12 (d, /= 8.1 Hz, 1H ), 6.23 (s, 1H), 6.16 (s, 2H), 4.28 – 4.35 (m, 2H), 1.32 – 1.37 (t, / = 7.2 Hz, 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 89501-90-6, A common heterocyclic compound, 89501-90-6, name is 1-Methyl-1H-pyrazole-3-sulfonyl chloride, molecular formula is C4H5ClN2O2S, 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: A solution of sodium sulfite (17.93g, 142.26 mmol) in H2O (100 ml) was stirred at room temperature for10 min. Sodium carbonate (23.90 g, 284.52 mmol)was added to the stirred solution.The resulting solution was stirred at 50 C for 10 minutes.cyclopropanesulfonyl chloride (20 g, 142.26 mmol) was added dropwise to thesolution and was stirred at 50 C for 2 hours. Thereaction mixture was evaporated to dryness and redissolved in EtOH (200 ml). The suspension was allowed to stir at roomtemperature for 20 min. The suspension was filtered and the filtrate evaporatedto afford a white solid, this was stirred with MeCN (50 ml) and thenfiltered to afford sodium cyclopropanesulfinicacid (13.70 g, 75 %) as a white solid. 1H NMR (400.132 MHz, DMSO d6)delta 1.38-1.31 (m, 1H), 0.27-0.24 (m,2H) and 0.08-0.03 (m, 2H).

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.

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. 1353100-91-0, name is Ethyl 3-bromo-1H-pyrazole-4-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., SDS of cas: 1353100-91-0

Example 102 Synthesis of ethyl 3-bromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazole-4-carboxylate. To a solution of ethyl 3-bromo-1H-pyrazole-4-carboxylate (547 mg, 2.5 mmol) and NaH (150 mg, 3.75 mmol, 60% oil) in THF (5 mL) and under N2 was added SEMCl (458 mg, 2.75 mmol) at 0 C. The reaction mixture was stirred at RT for 2 h. The reaction was quenched with H2O (30 mL) and extracted with EtOAc (30 mL*2). The combined organic layers were washed with brine, dried over Na2SO4 and concentrated in vacuo to afford ethyl 3-bromo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazole-4-carboxylate as a yellow oil (873 mg, yield: 99%) and a mixture of N1 and N2 regioisomers. ESI-MS [M+H]+: 350.1.

According to the analysis of related databases, 1353100-91-0, the application of this compound in the production field has become more and more popular.

Related Products of 16617-46-2, These common heterocyclic compound, 16617-46-2, name is 3-Amino-1H-pyrazole-4-carbonitrile, 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.

Step 1. A solution of 5-amino-1H-pyrazole-4-carbonitrile (10 g, 92.51 mmol, 1.00 equiv) in formamide (80 mL) was stirred under nitrogen at 165 ¡ãC for 5 h. The reaction mixture was cooled to room temperature and the solid was collected by filtration. The filter cake was washed first with 20 mL of water then 20 mL of methanol and dried to yield 9.5 g (76percent) of 1H-pyrazolo[3,4-d]pyrimidin-4-amine as a white solid.

Statistics shows that 3-Amino-1H-pyrazole-4-carbonitrile is playing an increasingly important role. we look forward to future research findings about 16617-46-2.

31108-57-3, name is 1H-Pyrazole-4-carbonitrile, 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 C4H3N3

3-(3-(4-(chloromethyl)benzyl)isoxazol-5-yl)pyridin-2 -amine (Intermediate B, 80mg, 0.27mmol) and lH-pyrazole-4-carbonitrile (99mg, l .07mmol) were dissolved in NMP (lml). Potassium 2- methylpropane-2-olate (1M in THF, 0.80mL, 0.80mmol) was added and the mixture was stirred for 5min at 60C. The cooled reaction mixture was directly purified by column chromatography (Si02, hexane/ethyl acetate). Fraction containing the product were concentrated under reduced pressure and further purified by HPLC to yield l-(4-((5-(2-aminopyridin-3-yl)isoxazol-3-yl)methyl)benzyl)-lH- pyrazole-4-carbonitrile (66mg, O. l9mmol, 69%) as a white solid. 400 MHz 1 H N R (CDCl3) d 8.13 (dd, J= 5.0, 1.8 Hz, 1H), 7.79 (dd, J= 18.1, 0.7 Hz, 2H), 7.69 (dd, J= 7.7, 1.8 Hz, 1H), 7.35 – 7.25 (m, 2H), 7.27 – 7.17 (m, 2H), 6.70 (dd, J= 7.7, 4.8 Hz, 1H), 6.25 (s, 1H), 5.43 (s, 2H), 5.30 (s, 2H), 4.05 (s, 2H). MS: 357.3 [M+H]+.

The synthetic route of 31108-57-3 has been constantly updated, and we look forward to future research findings.