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Water → 2,6-dichloro-N-(2-chloroethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,6-Dichlorobenzoyl chloride | HCID 78392 | — |
| 反応物 | 2-Chloroethylamine hydrochloride | HCID 9793737 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,6-dichloro-N-(2-chloroethyl)benzamide | HCID 15096972 | 68.8% |
反応手順
To a stirred (vigorously) mixture of 17.4 parts of 2-chloroethanamine hydrochloride, 20.7 parts of potassium carbonate and 225 parts of water was added dropwise a mixture of 31.3 parts of 2,6-dichlorobenzoyl chloride and 120 parts of dichloromethane at room temperature: slightly exothermic reaction. Upon completion, stirring at room temperature was continued for one hour. The organic phase was separated and the aqueous phase was extracted with dichloromethane. The combined organic phases were washed with water, dried, filtered and evaporated. The residue was crystallized from methylbenzene. The product was filtered off and dried, yielding 25.8 parts (68.8%) of 2,6-dichloro-N-(2-chloroethyl)benzamide; mp. 113.8° C. (intermediate 30).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05057525 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-73df445bc2dd411ba963a40e2193eb22 |
| 出典メモ | uspto-grants-1991_10 |