Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Chlorosulfonic acid → 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonyl chloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Chlorosulfonic acid | HCID 24638 | — |
| 반응물 | 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 19375487 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonyl chloride | HCID 11346737 | 45% |
반응 단계
A solution of 3-acetyl-2,3,4,5-tetrahydro-1H-3-benzazepine (4.0 g, 0.021 mol) in dichloromethane (25 ml) was added dropwise to a stirred solution of chlorosulphonic acid in dichloromethane (25 ml) at −70° C. under argon. After warming to room temperature, the reaction was stirred for 18 h before being quenched in ice/water (200 ml). The resulting mixture was extracted with ethyl acetate (3×100 ml), dried (Na2SO4) and the solvent evaporated in vacuo to give the title compound (2.74 g, 45%) as a pale yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07429579B2 |
| 출처 데이터셋 | uspto-grants-2008_09 |
| ORD ID | ord-c8f98f0a35ae4a16a55654d6994ad5bc |
| 출처 메모 | uspto-grants-2008_09 |