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Thiophosgene → 4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophosgene | HCID 10040 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(2,5-Dichlorophenoxy)-3-fluoroaniline | HCID 28972706 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylisothiocyanate | HCID 59797663 | 97.4% |
反応手順
4-(2,5-Dichloro-phenoxy)-3-fluoro-phenylamine (1.36 g, 5 mmol) was dissolved in 150 ml of chloroform and 100 ml of saturated aqueous sodium bicarbonate was added. To this biphasic mixture was added dropwise a solution of thiophosgene (0.39 ml, 5 mmol) in 30 ml of chloroform at room temperature with vigorous stirring. The mixture was stirred vigorously for 1 hour at room temperature. The bottom layer of the mixture was separated, and the aqueous layer was extracted twice with CHCl3. The combined organic solution was washed with water, dried over Mg2SO4 and evaporated to give 1.53 g (97.4%) of crude product used for next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07429667B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-b997bf5941b9465ca8966a1a87240e14 |
| 出典メモ | uspto-grants-2008_09 |