Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Water → 4-Chloro-2-fluoro-5-propargylthioaniline
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 3-Chloro-1-propyne | HCID 12221 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Benzenethiol, 5-amino-2-chloro-4-fluoro- | HCID 11019406 | — |
| 촉매 | Benzyltributylammonium chloride | HCID 159952 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 4-Chloro-2-fluoro-5-propargylthioaniline | HCID 13488953 | 31.9% |
반응 단계
To a mixture of 5-amino-2-chloro-4-fluorothiophenol (8.4 g), sodium hydroxide (3 g), water (80 ml), diethyl ether (40 ml) and tributylbenzylammonium chloride (0.1 g), propargyl chloride (5.2 g) was dropwise added at room temperature (ca. 20° to 25° C.), and the resultant mixture was stirred at the same temperature for 3 hours. The water layer was separated and extracted with ether. The ether extract was combined with the ether layer, washed with water, dried and concentrated under reduced pressure. The residue was crystallized from methanol to give 3.25 g of 4-chloro-2-fluoro-5-propargylthioaniline. M.P., 58°-59.5° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04933480 |
| 출처 데이터셋 | uspto-grants-1990_06 |
| ORD ID | ord-d883830b8db745099a552bd4d1283f0d |
| 출처 메모 | uspto-grants-1990_06 |