Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethylformamide dimethyl acetal → (E)-ethyl 4-(2-(dimethylamino)vinyl)-2-(methylthio)pyrimidine-5-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethylformamide dimethyl acetal | HCID 78373 | — |
| 반응물 | Ethyl-2-methylthio-4-methyl-5-pyrimidine carboxylate | HCID 188208 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | (E)-ethyl 4-(2-(dimethylamino)vinyl)-2-(methylthio)pyrimidine-5-carboxylate | HCID 86657908 | 62% |
반응 단계
4-Methyl-2-methylsulfanyl-pyrimidine-5-carboxylic acid ethyl ester 3 (18.0 g, 84.8 mmol) was dissolved in DMF (50 mL), N,N-Dimethylformamidedimethylacetal (22.5 mL, 170 mmol) and stirred at reflux for 3 hours. Then mixture was concentrated, the residue was dissolved in TCM, washed with water, dried, filtered, and concentrated. The product was purified by crystallization from ether to yield in a colorless solid (14.0 g, 52.5 mmol, 62%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08530650B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-dc974b9b448b4f40ae01977f5f513159 |
| 출처 메모 | uspto-grants-2013_09 |