反应详情

温度

50 °C

A mixture of dimethyl malonate (42.6 g, 322.73 mmol, 4.00 equiv) and potassium carbonate (22.3 g, 161.59 mmol, 2.00 equiv) in N,N-dimethylformamide (200 mL) was stirred for 30 min at 50° C. A solution of 1-bromo-4-(bromomethyl)benzene (20 g, 80.65 mmol, 1.00 equiv) in N,N-dimethylformamide (80 mL) was then added dropwise with stirring to the reaction mixture. The resulting solution was stirred at 50° C. for 2 h. Water (100 mL) was added and the mixture was extracted with 1×400 mL of ethyl acetate. The organic layer was washed with 2×100 mL of brine, dried over anhydrous sodium sulfate and concentrated under vacuum to give 22 g (91%) of dimethyl 2-(4-bromobenzyl)malonate as a white solid. LC-MS: (ES, m/z): 301 [M+H]+, 126, 120.

1. stirringwith stirring to the reaction mixture
2. stirringThe resulting solution was stirred at 50° C. for 2 h
3. extractionthe mixture was extracted with 1×400 mL of ethyl acetate
4. washThe organic layer was washed with 2×100 mL of brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated under vacuum