反应详情

2-(2,4-Dichlorobenzoyl)cyclohexane-1,3-dione (2.85 g, 0.01 ml) was stirred as a suspension in 25 ml anhydrous ether. Diazomethane, generated from Diazald™ (50 ml, 0.02 mol) was added at 0° at a rate slow enough to control effervescence. The resulting solution was stirred for an hour and the solvent allowed to evaporated under a stream of nitrogen in a beaker. The resulting oil was dissolved in ether and washed twice with saturated aqueous K2CO3. Evaporation of the solvent under reduced pressure yielded a solid (1.0 g, 35%, m.p. 81°-86° C.), the nuclear magnetic, infrared and mass spectra of which were consistent with the structure.

1. additionwas added at 0° at a rate slow enough
2. customto evaporated under a stream of nitrogen in a beaker
3. dissolutionThe resulting oil was dissolved in ether
4. washwashed twice with saturated aqueous K2CO3
5. customEvaporation of the solvent under reduced pressure