反应详情

3 g. of magnesium oxide are added to a solution of 2.87 g. (0.01 mmoles) of 1-methyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2 H-1,4-benzodiazepine-2-one in 30 ml. of chloroform, and a solution of 1.2 ml. (0.018 moles) of chloroacetyl chloride in 4 ml. of chloroform is added to the vigorously stirred mixture. After 3 hours of stirring at room temperature the magnesium salt is filtered off, washed with 20 ml. of chloroform, and the filtrate is evaporated to dryness under reduced pressure. The residue is crystallized from acetone. 2.68 g. (8.14 %) of 1-methyl-4-chloroacetyl-5-phenyl-7-chloro-1,3,4,5-tetrahydro-2H-1,4-benzodiazepine-2-one are obtained; m.p.: 197°-200° C.; Rf2 = 0.5.

1. filtrationis filtered off
2. washwashed with 20 ml
3. customof chloroform, and the filtrate is evaporated to dryness under reduced pressure
4. customThe residue is crystallized from acetone