반응 #40886

반응 방정식

Water

ethyl acetate

2-bromo-1-phenylethanone

→

title compound

수율 50.0%

1—Ethyl [2-oxo-3-(2-oxo-2-phenylethyl)cyclohexyl]acetate

수율 50.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.STIRRINGto stir for a further 24 h
2. 2
   세척washed with water
3. 3
   추출The aqueous fraction was re-extracted three times with ethyl acetate
4. 4
   세척the combined organic fractions washed three times with water
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated in vacuo

실험 절차

Intermediate 2 (667 mg, 2.81 mmol) was dissolved in dimethylformamide (14 ml), 2-bromo-1-phenylethanone (560 mg, 2.81 mmol) was added and the reaction stirred for 24 h at room temperature. Water (5 ml) was added and the reaction allowed to stir for a further 24 h. The mixture was then diluted with ethyl acetate (100 ml) and washed with water. The aqueous fraction was re-extracted three times with ethyl acetate and the combined organic fractions washed three times with water, then dried over sodium sulfate, filtered and concentrated in vacuo. Column chromatography (10-20% ethyl acetate/hexanes) provided the title compound as a pale yellow oil (428 mg, 50%).

출처