Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Isopropyl chloroformate → 2,6-Dichloropyridine-3-carboxamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Isopropyl chloroformate | HCID 7917 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 2,6-Dichloronicotinic acid | HCID 854047 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2,6-Dichloropyridine-3-carboxamide | HCID 22142778 | 109.9% |
반응 단계
A mixture of 2,6-dichloro-3-carboxypyridine (5.73 g, 30 mmole) and N-methylmorpholine (3.6 ml, 33 mmole) in dichloromethane (100 ml) was stirred in an ice-bath for 5 min. Isopropyl chloroformate (4.28 ml, 33 mmole) was added the reaction mixture at 0° C. The reaction mixture was stirred for 30 min and then bubbled with pure ammonia gas for 2 min. and stirred overnight at room temperature. The crude was concentrated under reduced pressure and sodium bisulfate (0.5M, 35 ml) was added with stirring. The aqueous solution was extracted with ethyl acetate (3×40 ml). The organics was washed with water and brine and dried with sodium sulfate to give yellow crude product (6.3 g, 50% pure).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07425557B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-921126856bfb47c2a39e9b6cebd883a0 |
| 출처 메모 | uspto-grants-2008_09 |