Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diethyl Ether → 1,4-Dichloroisoquinoline-7-sulfonyl chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 4-Chloro-1-hydroxy-7-isoquinolinesulfonyl chloride | HCID 16658351 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 1,4-Dichloroisoquinoline-7-sulfonyl chloride | HCID 16658294 | 84.2% |
반응 단계
Phosphorus oxychloride (POCl3) (9.65 mL, 103.5 mmol) was added to a stirred suspension of 4-chloro-7-chlorosulphonyl-1-(2H)-isoquinolone (22.1 g, 79.6 mmol) in MeCN (500 mL) at room temperature and the mixture was then heated at reflux for 15 h. On cooling, the MeCN solution was decanted from the insoluble sludge and evaporated in vacuo. The residue was extracted with hot EtOAc and evaporated to leave a solid which was stirred with Et2O (1.2 L) at room temperature overnight. The ethereal solution was decanted from the insoluble material and evaporated in vacuo to give 7-chlorosulphonyl-1,4-dichloroisoquinoline (20 g, 67 mmol) as a pale yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06248738B1 |
| 출처 데이터셋 | uspto-grants-2001_06 |
| ORD ID | ord-c24f4ee4e02941e2b8badf179b698531 |
| 출처 메모 | uspto-grants-2001_06 |