Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide → 4-(3-Amino-4-cyano-pyrazol-1-ylmethyl)-benzoic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl 4-(bromomethyl)benzoate | HCID 256687 | — |
| 반응물 | HCID 178510443 | HCID 178510443 | — |
| 용매 | Acetone diethylether | HCID 21584533 | — |
| 생성물 | 4-(3-Amino-4-cyano-pyrazol-1-ylmethyl)-benzoic acid methyl ester | HCID 66622281 | 24% |
반응 단계
To a solution of 3-amino-1H-pyrazole-4-carbonitrile (1.211 g, 11.21 mmol) in anhydrous DMF (20 ml) K2CO3 (5.414 g, 39.24 mmol) was added. The suspension was stirred 5 min at room temperature and treated with p-bromomethylbenzoic acid methyl ester (2.568 g, 11.21 mmol), stirred for 2.5 hrs at 100° C., cooled and filtered. Filtrate was evaporated to form an oily residue, which was dissolved in a mixture Et2O-acetone and kept overnight at −10° C. A crystalline material was formed which was triturated with hot EtOAc, again kept overnight at −10° C. and was collected by filtration to form the title compound 95 (675 mg, 24% yield). LRMS: 256.3 (calc.), 257.3 (found).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07253204B2 |
| 출처 데이터셋 | uspto-grants-2007_08 |
| ORD ID | ord-95f05e6e9d77478ca08eb5d511184661 |
| 출처 메모 | uspto-grants-2007_08 |