Chloroacetyl chloride → HCID 20554414, compound

Participants

Reaction Conditions

Reaction Steps

28 g (250 mmol) of chloroacetyl chloride and 28 g (250 mmol) of sodium carbonate are added to a solution of 20 g (63 mmol) of 6-ethyl-2-phenyl-5,6-dihydropyrimido[4,5-b][1,5]benzodiazepin-5-one in 500 ml of absolute toluene. The mixture is stirred for 20 hours at 100° C. The solvent is removed on a rotary evaporator, and the residue is neutralized with 2 N-hydrochloric acid. The mixture is extracted with chloroform, and the organic phase is washed with water, dried and concentrated in vacuo. The residue which remains is recrystallized from isopropanol; yield: 19.2 g (77%), m.p. 147° to 148° C.

Provenance & Evidence