Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 1-Benzyl-5-chloro-3-chloromethylcinnolin-4(1H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Methanesulfonyl chloride | HCID 31297 | — |
| 반응물 | 1-Benzyl-5-chloro-3-hydroxymethylcinnolin-4(1H)-one | HCID 67267209 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-Benzyl-5-chloro-3-chloromethylcinnolin-4(1H)-one | HCID 67267510 | 59% |
반응 단계
To 0.42 g (1.4 mmol) of 1-benzyl-5-chloro-3-hydroxymethylcinnolin-4(1H)-one in 25 mL of dichloromethane at 0° C. was added 0.97 mL (7.0 mmol) of triethylamine and 0.33 mL (4.2 mmol) of methanesulfonyl chloride. The reaction was allowed to warm to room temperature and stirred for 5 h. The reaction was concentrated by rotary evaporation and was subsequently dissolved in dichloromethane and concentrated onto silica gel. The crude material was purified by flash chromatography eluting with a 33-50% ethyl acetate/hexanes gradient mixture to give 0.26 g (59%) of the title compound as an off-white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07897607B2 |
| 출처 데이터셋 | uspto-grants-2011_03 |
| ORD ID | ord-41e6e0f12f044669af05aab064d12633 |
| 출처 메모 | uspto-grants-2011_03 |