化工社化工社 化学情報印刷レポート · 研究参考用
Water → 4-Chloro-2-fluoro-5-propargylthioaniline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Chloro-1-propyne | HCID 12221 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Benzenethiol, 5-amino-2-chloro-4-fluoro- | HCID 11019406 | — |
| 触媒 | Benzyltributylammonium chloride | HCID 159952 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 4-Chloro-2-fluoro-5-propargylthioaniline | HCID 13488953 | 31.9% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04933480 |
| 出典データセット | uspto-grants-1990_06 |
| ORD ID | ord-d883830b8db745099a552bd4d1283f0d |
| 出典メモ | uspto-grants-1990_06 |