反应详情

t-Butyl chloroacetate (13.0g, prepared according to Org. Synth., Coll.Vol. 4, 263) was added dropwise to a stirred mixture of N-hydroxyphthalimide (14.2g), triethylamine (23.0g), and dimethylformamide (30ml), and the resulting mixture was stirred for 4 hr. The mixture was poured into water (500 ml), and the precipitated solid was collected, washed with water, and dried. Recrystallisation from ethanol gave N-t-butoxycarbonylmethoxyphthalimide (17.26g, 72%); m.p. 145.6°; τ values (DMSO-d6) 2.09 (4 Ar-H), 5.28 (CH2), 8.56 (But).

1. customthe precipitated solid was collected
2. washwashed with water
3. customdried
4. customRecrystallisation from ethanol