反应详情

温度

0 °C

A solution of dimethyl malonate (13.2 g), 4-bromobenzylbromide (5.4 g) in DMF (200 mL) was treated with NaH (4 g, 60% in mineral oil). The mixture was stirred for 5 min at 0° C. and 20 min at room temperature and then quenched with 10 mL of AcOH slowly. The mixture was concentrated under vacuum and the residue was dissolved in 200 mL of 1:1 EtOAc/hexane, and filtered through a pad of silica gel. The filtrate was concentrated and the excess dimethyl malonate was removed under vacuum at 70° C. to provide the title compound as a yellow oil.

1. customquenched with 10 mL of AcOH slowly
2. concentrationThe mixture was concentrated under vacuum
3. dissolutionthe residue was dissolved in 200 mL of 1:1 EtOAc/hexane
4. filtrationfiltered through a pad of silica gel
5. concentrationThe filtrate was concentrated
6. customthe excess dimethyl malonate was removed under vacuum at 70° C.