反应详情

A solution of glycine methyl ester hydrochloride (5.00 g, 39.8 mmol) in 80 ml methyl isobutyl ketone is treated with 12.6 g of sodium carbonate and the mixture stirred overnight at RT. Next, a solution of 2-bromo-1-(4-chlorophenyl)ethanone (8.37 g, 35.8 mmol) in 40 ml methyl isobutyl ketone is added dropwise to this suspension. The mixture is stirred for 1 hr more at RT, then the solid is suction-filtered and washed with 55 ml methyl isobutyl ketone. The filtrate is acidified with 12 ml of 6 N hydrochloric acid, then treated with 6.4 ml isopropanol. The precipitated solid is filtered off at the pump, washed with a little methyl isobutyl ketone, then stirred in 240 ml of acetonitrile and again suction-filtered. 3.41 g (34% of theory) of the pure title compound are thus obtained.

1. stirringThe mixture is stirred for 1 hr more at RT
2. filtrationthe solid is suction-filtered
3. washwashed with 55 ml methyl isobutyl ketone
4. additiontreated with 6.4 ml isopropanol
5. filtrationThe precipitated solid is filtered off at the pump
6. washwashed with a little methyl isobutyl ketone
7. stirringstirred in 240 ml of acetonitrile
8. filtrationagain suction-filtered