Category: 1280210-79-8

Electric Literature 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.

3 -(Bromomethyl)- 1,1 -difluoro-cyclobutane (505 mg, 2.73 mmol) was added dropwisc over 15 mm, to a mixture of tert-butyl 4,6-dihydro-2H-pyrrolo[3,4- c]pyrazole-5-carboxylate (560 mg, 2.67 mmol), cesium carbonate (1.39 g, 4.28 mmol) and DMF (5 mL) at 0 C. The reaction mixture was allowed to warm to ambient temperature and stirred for 18 h. The solvent was concentrated and the material was partitioned betweenwater (50 mL) and EtOAc. The aqueous layer was washed with EtOAc (2 x 30 mL). The combined organic layers were washed with brine, dried (MgSO4), and the solvent was concentrated. Purification (FCC, Si02 using ether) provided the title compound (344 mg, 41%). ?H NMR (300 MHz, CDC13) 3 = 7.10 (d, J = 10.0 Hz, 1H), 4.50 -4.37 (m, 4H), 4.18 (d, J = 5.5 Hz, 2H), 2.78-2.56 (m, 3H), 2.47-2.25 (m, 2H), 1.50 (s, 9H); [M+H] = 314.26.

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

Synthetic Route of 1280210-79-8, 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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows.

2D (3.5 g, 16.7 mmol) was dissolved in tetrahydrofuran (35 mL)Cooled to 0 C,60% sodium hydride (1.0 g, 25.4 mmol) was added,After reaction for 30 minutes, methylsulfonyl chloride (2.9 g, 25.4 mmol) was added and reacted for 1 hour.The reaction mixture was quenched with water (10 mL) and extracted with ethyl acetate (50 mL x 2). The organic layers were combined and the organic layer was dried over anhydrous sodium sulfate and concentrated. The residue was purified by silica gel column chromatography (petroleum ether / Ethyl acetate (v / v) = 1: 1) to give 2E as a white solid (2.1 g, yield 44%).

The chemical industry reduces the impact on the environment during synthesis tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate. I believe this compound will play a more active role in future production and life.

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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., COA of Formula: C10H15N3O2

Synthesis of 244-A. To a solution of tert-butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)- carboxylate (1.40 g, 6.70 mmol) in DCM (10 mL) was added TFA (3 mL) dropwise under ice bath. Then the solution was stirred at room temperature 1 h. The solvent was removed in vacuo to give 244- A as a crude product

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 1280210-79-8.

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

under nitrogen protection, Intermediate 2(1000 mg, 4.78mmol) is dissolved in N, N – dimethyl formamide(15ml), lowering the temperature to -15 C, sodium bis(trimethylsilyl)amide (4.78 ml, 2 mol/L, 9.56mmol), was added stirring 30 minutes, will S – tetrahydrofuran -3 – sulfonyl chloride (1.39g, 8.13mmol) is added in the reaction solution, to maintain this temperature reaction is 16 hours. The end of the reaction, raising the temperature to 0 C, adding water to the reaction solution (20 ml) quenching the reaction, ethyl acetate (20mL ¡Á 2) extraction, the combined organic layer, drying with anhydrous sodium sulfate, concentrated, re-dissolved in tetrahydrofuran (20 ml) in, cooling to -10 C to 0 C. Adding 3rd butanol potassium (85 mg, 0.76mmol), this temperature is kept under 24 hours reaction. The end of the reaction, by adding saturated ammonium chloride solution (10 ml), water (10 ml), ethyl acetate (20mL ¡Á 3) extraction, the combined organic layer, drying with anhydrous sodium sulfate, concentrated. Silica gel column chromatography separation and purification of the residue (petroleum ether/ethyl acetate (v/v)=5:1), to obtain white solid5a(810 mg, 62.3% yield).

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

Related Products of 1280210-79-8, These common heterocyclic compound, 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-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.

To a solution of tert-butyl 4,6-dihydropyrrolo[3,4- c]pyrazole-5(2H)-carboxylate (250 mg, 1.2 mmol) in DMF (5 mL) was added NaH (96 mg, 2.4 mmol (60% in mineral oil)), with the reaction mixture being cooled with an ice bath. The resulting mixture was stirred at room temperature for 1 h, whereupon iodoethane (374 mg, 2.4 mmol) was added, and the resulting reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then diluted with water (10 mL) and extracted with EtOAc (10 mL x 3). The combined organic layers were washed with brine (10 mL x 3), dried over anhydrous Na2S04 and then concentrated in vacuo to give 135 and 135-A as a crude product. MS 238.2 [M + H]+. (0141) [0090] Synthesis of 136 and 136- A. To a solution of 135 and 135-A (1.2 mmol, crude product from last step) in DCM (6 mL) was added TFA (2 mL) dropwise while the reaction mixture was cooled with an ice bath. The reaction mixture was stirred at room temperature 1 h, whereupon the solvent was removed in vacuo to give 136 and 136-A as a crude product which was used in the next step without further purification. MS 138.2 [M + H]+. (0142) [0091] Synthesis of 137. A mixture of 136 and 136-A (1.2 mmol, crude product from last step) and A3 (491 mg, 1.0 mmol) in DMSO (10 mL) was stirred at room temperature for 10 min, then Na2C03 (848 mg, 8.0 mol) was added, and the reaction mixture was stirred at room temperature for 2 h. The reaction mixture was then diluted with water (20 mL) and extracted with EtOAc (20 mL x 3). The combined organic layers were washed with brine (20 mL x 3), dried over anhydrous Na2S04 and then concentrated in vacuo. The crude residue was purified by column chromatography on silica gel (DCM : MeOH = 100 : 1 ~ 50 : 1) to give a crude product which was a mixture of the regioisomers 137 and 137-A. The crude product was further purified by Prep-TLC (DCM : MeOH = 30 : 1) to give 137 (150 mg, 36%) as a yellow solid. MS 415.1 [M + H]+.

The synthetic route of 1280210-79-8 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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C10H15N3O2

Synthesis of 257-A and 258-A. A mixture of tert-butyl 4,6-dihydropyrrolo[3,4- c]pyrazole-5(2H)-carboxylate (314 mg, 1.50 mmol), Cs2CO3 (978 mg, 3.00 mmol) and iodomethane (320 mg, 2.25 mmol) in DMF (6 mL) was stirred at room temperature for 16 h. The mixture was diluted with water (18 mL), extracted with EtOAc (10 mL ¡Á 3). The combined organic layer was washed with brine (10 mL ¡Á 3), dried over anhydrous Na2SO4 and then concentrated in vacuo. The residue was purified by column chromatography on silica gel (DCM : MeOH = 100 : 1 ~ 50 : 1) to give 257-A and 258-A (270 mg, 81%) as a yellow solid.

According to the analysis of related databases, 1280210-79-8, the application of this compound in the production field has become more and more popular.

Synthetic Route of 1280210-79-8, 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 1280210-79-8 as follows.

Intermediate 2 (3.5 g, 16.7 mmol) was dissolved in tetrahydrofuran (35 ml), and sodium hydride (1.0 g, 60%, 25.4 mmol) was added at 0C, followed by reaction for 30 min. Methylsulfonyl chloride (2.9 g, 25.4 mmol) was added, followed by reaction for 1 hour. The reaction was quenched by addition of water (10 ml) to the reaction solution, which was extracted with ethyl acetate (50 ml*2). The organic layers were combined, dried over anhydrous sodium sulfate, concentrated, and purified by silica gel column chromatography (petroleum ether/ethyl acetate (v/v) = 1:1), to obtain a white solid 3a (2.1 g, yield 44%).

According to the analysis of related databases, 1280210-79-8, the application of this compound in the production field has become more and more popular.

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. 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate, This compound has unique chemical properties. The synthetic route is as follows., Recommanded Product: tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate

To 4,6-dichloropyrimidine (674 mg, 4.52 mmol) in dimethylformamide (3.4 ml) under an atmosphere of argon was added tert-butyl 2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-carboxylate (946 mg, 4.52 mmol) and cesium carbonate (1.47 g, 4.52 mmol) and the reaction stirred overnight at room temperature. The reaction was poured onto water (25 ml) and stirred for 60 minutes. The precipitate was filtered and purified by HPLC (Method 20) to yield 748 mg (100% purity, 51 % yield) of the desired product. LC-MS (Method 10): Rt = 2.10 min; MS (ESIpos): m/z = 322 [M+H]+1H-NMR (600 MHz, dimethylsulfoxide-d6) delta [ppm]: 1.466 (16.00), 4.400 (1.20), 4.427 (1.38), 4.456 (1.47), 4.477 (1.29), 7.884 (0.67), 7.903 (0.79), 8.467 (0.69), 8.493 (0.62), 8.925 (1.44).

According to the analysis of related databases, 1280210-79-8, the application of this compound in the production field has become more and more popular.

1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-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. Safety of tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-carboxylate

Under N2 protection and a condition free of water and oxygen, Intermediate 2 (604 mg, 2.87 mmol) wasdissolved in tetrahydrofuran (20 ml), which was cooled to 0C, and sodium hydride (180 mg, 60 wt%, 4.5 mmol) wasadded, followed by stirring for 30 min. Cyclopropylsulfonyl chloride (1.27 g, 9.0 mmol) was added dropwise, and thetemperature was allowed to rise spontaneously to room temperature, followed by reaction for 1 hour. The reaction was quenched by addition of water (20 ml) to the reaction solution, which was then extracted with ethyl acetate (20 ml32).The organic phases were combined, dried over anhydrous sodium sulfate, concentrated, re-dissolved in 5 ml tetrahydrofuran,and cooled to -10C to 0C. Potassium t-butoxide (36 mg, 0.32 mmol) was added, and the reaction was allowedto proceed for 28 hours at this temperature. After the reaction was completed, an aqueous solution of citric acid (1 ml,15%) was added, and water (10 ml) was added. The solution was extracted with ethyl acetate (20 mL33). The organicphases were combined, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gelcolumn chromatography (petroleum ether/ethyl acetate (v/v) = 2:1) to obtain a white solid 1a (660 mg, yield 73%).

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

Electric Literature of 1280210-79-8, These common heterocyclic compound, 1280210-79-8, name is tert-Butyl 4,6-dihydropyrrolo[3,4-c]pyrazole-5(2H)-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.

INTERMEDIATE 12; 2-(( clopropylsxrffonylV2.4.5.6-tetrahvdropyrrolof3.4-c]pyrazole trifluoroacetic acid salt Step A: fe^Bu 2-(cyclopen sulfonYl>2.6-^carboxylateTo a suspension of sodium hydride (60% dispersion in oil, 1.55 g, 38.7mmol) in anhydrous acetonitrile (200 mL) was added to terf-butyl 2,6-dihyclropyrrolo[3,4-c]pyrazole- 5(4H)-carboxylate (5.3 g, 25.5 mmol) in one portion under nitrogen at room temperature. The reaction mixture was stirred at room temperature for 2 h. To the resulting white suspension was slowly added cyclopropanesulfonyl chloride (6.9 g, 49.1 mmol) and the mixture was stirred at room temperature for 18 h, quenched with water (120 mL) and the layers were separated. The aqueous layer was then extracted with dichloromethane (2 x 100 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The crude material was purified on silica chromatography (300 g Biotage column) and eluted with 15-80% ethyl acetate in hexanes to yield the title compound and ter/-butyl 1- (cyclopentyisulfonyl)-2,6-dihydropyrrolo[3,4-c]pyrazole-5(4H)-carboxylate as a white solid. LC/MS: 314.2(M+1).

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