反应详情

温度

0 °C

Concentrated H2SO4 (38.5 mL) was added dropwise via addition funnel to diethyl 2-(2-methyl-2-phenylpropanoyl)malonate (22.1 g, 72.1 mmol) cooled to 0° C. The reaction mixture was stirred for 2 hours at 0° C. and then poured into a flask containing ice, diluted with 400 mL of EtOAc, added to a separatory funnel, partitioned with water, washed 2 times with 100 mL of water, separated, dried over Na2SO4, and concentrated in vacuo to give the title compound (10.82 g) as a white amorphous solid after flash chromatography. MS (m/z)=261 (M+H)+.

1. additionpoured into a flask
2. additioncontaining ice
3. additionadded to a separatory funnel
4. custompartitioned with water
5. washwashed 2 times with 100 mL of water
6. customseparated
7. dry with materialdried over Na2SO4
8. concentrationconcentrated in vacuo