참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 1H-Indazole-4-carbonitrile | HCID 24729347 | — |
| 반응물 | Methanesulfonic acid 3-chloro-1-phenyl-propyl ester | HCID 57985877 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 1-(3-chloro-1-phenyl-propyl)-1H-indazole-4-carbonitrile | HCID 58088445 | 36.8% |
반응 단계
Sodium hydride (0.092 g, 60% in oil) was added to a solution of 4-cyanoindazole (0.300 g) in N-methylpyrrolidinone (5 mL) and the reaction mixture was stirred at room temperature for 30 minutes. Methanesulfonic acid 3-chloro-1-phenyl-propyl ester (0.573 g) was added followed by 3 ml more of N-methylpyrrolidinone. The reaction mixture was stirred for an additional 6 hours at room temperature. The reaction mixture was partitioned between water and ethyl acetate, and the organic layer was washed with water, then with brine, and dried (MgSO4). Evaporation to dryness gave a residue which was purified by column chromatography on silica gel using ethyl acetate-hexane (1:9) to give 1-(3-chloro-1-phenyl-propyl)-1H-indazole-4-carbonitrile (0.228 g) as a foam, (M+H=297).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07863305B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_01 |
|---|
| ORD ID | ord-70e31736f1c04e8aadfd794e87fa6569 |
|---|
| 출처 메모 | uspto-grants-2011_01 |
|---|