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Water → 3-Chloro-2-[2-chloro-4-(methanesulfonyl)benzoyl]cyclohex-2-en-1-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Oxalyl chloride | HCID 65578 | — |
| 反応物 | Sulcotrione | HCID 91760 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Chloro-2-[2-chloro-4-(methanesulfonyl)benzoyl]cyclohex-2-en-1-one | HCID 14279982 | 70.1% |
反応手順
2-(2-Chloro-4-methanesulfonylbenzoyl)-cyclohexane-1,3-dione [9.8 g, 30 millimole (mmol)] was dissolved in 100 ml methylene chloride and stirred at room temperature. To this solution was added oxalyl chloride (5.7 g, 45mmol) followed by dimethylformamide (0.5 ml) in portions small enough to control effervescence. The resulting solution was stirred for 4 hours and then poured into water and extracted with methylene chloride. The organic layer was washed again with water, saturated K2CO3 solution andthen dried with MgSO4 and the solvent evaporated to yield 3-chloro-2(2-chloro-4-methanesulfonylbenzoyl)cyclohex-2-enone (7.3 g, 70%)as an oil which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04775411 |
| 出典データセット | uspto-grants-1988_10 |
| ORD ID | ord-71c1f3a15f6a404485c9b9fa6f1f9026 |
| 出典メモ | uspto-grants-1988_10 |