반응 #62788

반응 방정식

water

oxalyl chloride

2-(2-Chloro-4-methanesulfonylbenzoyl)-cyclohexane-1,3-dione

dimethylformamide

→

3-chloro-2-(2chloro-4-methanesulfonylbenzoyl)cyclohex-2-enone

수율 70.1%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.STIRRINGThe resulting solution was stirred for 4 hours
2. 2
   추출extracted with methylene chloride
3. 3
   세척The organic layer was washed again with water, saturated K2CO3 solution
4. 4
   건조dried with MgSO4
5. 5
   기타the solvent evaporated

실험 절차

2-(2-Chloro-4-methanesulfonylbenzoyl)-cyclohexane-1,3-dione (9.8 g, 30 millimole) was dissolved in 100 ml methylene chloride and stirred at room temperature. To this solution was added oxalyl chloride (5.7 g, 45 mmol) 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 and then dried with MgSO4 and the solvent evaporated to yield 3-chloro-2-(2chloro-4-methanesulfonylbenzoyl)cyclohex-2-enone (7.3 g, 70%) as an oil which was used without further purification.

출처