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4-Chloro-2-fluorophenyl isocyanate → 3-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 4-Chloro-2-fluorophenyl isocyanate | HCID 4558203 | — |
| 反応物 | Ethyl thiomorpholine-3-carboxylate | HCID 13604869 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | 3-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine | HCID 23343397 | 87.7% |
反応手順
An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04220465 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-95b0801eb1af422b91d722b853fc31cf |
| 出典メモ | uspto-grants-1980_09 |