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Dichloromethane → Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Methanesulfenyl chloride, trifluoro- | HCID 67900 | — |
| 反応物 | 1-Chloro-4-(isocyanomethyl)benzene | HCID 2757409 | — |
| 生成物 | Trifluoromethyl 1-chloro-N-(p-chlorobenzyl)thioformimidate | HCID 18930385 | 68% |
反応手順
Trifluoromethylsulfenyl chloride (4.0 g, 0.03 mol) is bubbled over 30 minutes into a solution of 4-chlorobenzylisonitrile (3.0 g, 0.02 mol) in methylene chloride, causing the formation of a white precipitate. The suspension is stirred for 16 hours at room temperature and filtered to remove solids. The white filter cake is washed with methylene chloride and solvent is removed under reduced pressure to obtain an amber oil. Bulb-to-bulb distillation of the oil (90°-100° C., 0.05 mmHg) gives the title product as a colorless oil (3.9 g, 68%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05468877 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-ad5fc0c2af754edcbfdc8a065345f3fb |
| 出典メモ | uspto-grants-1995_11 |