化工社化工社 化学情報印刷レポート · 研究参考用
Thiophosgene → 2-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | 3-Amino-2-fluorobenzotrifluoride | HCID 145569 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Fluoro-1-isothiocyanato-3-trifluoromethyl-benzene | HCID 83402407 | 91% |
反応手順
To a two phase solution of 2-fluoro-3-trifluoromethyl-phenylamine (2 g, 11.17 mmole) in dichloromethane (40 ml) and sodium bicarbonate (6.57 g, 78.19 mmole) in water (30 ml) at 0° C. was added dropwise a solution of thiophosgene (1.28 g, 11.17 mmole) in dichloromethane (10 ml). After 2 hrs, the organic layer was separated, washed sequentially with 1M NaHCO3, brine and water. The organic layer was dried over Na2SO4, filtered and concentrated to yield 2.2 g (91%) of product as a viscous liquid. MS (ESI+) m/z 221 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07723367B2 |
| 出典データセット | uspto-grants-2010_05 |
| ORD ID | ord-86d9f4c08ec9444695bc6c53d1535e34 |
| 出典メモ | uspto-grants-2010_05 |