Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
N,N-Diethylaniline → 2-Chloro-5-fluoro-1-methyl-1H-benzimidazole
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | N,N-Diethylaniline | HCID 7061 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 5-Fluoro-1-methyl-1H-benzo[d]imidazol-2(3H)-one | HCID 22028684 | — |
| 생성물 | 2-Chloro-5-fluoro-1-methyl-1H-benzimidazole | HCID 21985828 | — |
반응 단계
3.9 g 5-fluoro-1-methyl-1,3-dihydro-benzimidazol-2-one are suspended in 80 ml phosphorus oxychloride and the reaction mixture is stirred for 2 hours at reflux temperature. 50 ml diethylaniline are added. The reaction mixture is stirred for a further 10 minutes at reflux temperature and ice water is slowly added thereto. The product is extracted with dichloromethane and purified by chromatography (silica gel, cyclohexane, methylene chloride/acetone 20/1). 1.4 g product are obtained in the form of a solid. M.p.=138-141° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08592400B2 |
| 출처 데이터셋 | uspto-grants-2013_11 |
| ORD ID | ord-84405a598f584daaaf62ef93232152db |
| 출처 메모 | uspto-grants-2013_11 |