反应详情

温度

60 °C

A mixture of 2-(p-chlorophenyl)-N-(trifluoroacetyl)sarcosine (147.7 g, 0.50 mol) in acetonitrile is treated dropwise with α-chloroacrylonitrile (54.7 g, 0.62 mol) and acetic anhydride (153 g, 1.5 mol), stirred vigorously, treated dropwise with triethylamine (58.1 g, 0.57 mol) at 56°-60° C. over a 11/4 hour period, heated at 60° C. for 16 hours and concentrated in vacuo to give a residue. The residue is partitioned between ethyl acetate and water. The organic phase is concentrated in vacuo to afford an amber solid residue. Said solid is purified by flash chromatography (silica; ethyl acetate/hexanes) and recrystallized from methanol to give the title product as a pale yellow solid, mp 129.5°-130.5° C.

1. concentrationconcentrated in vacuo
2. customto give a residue
3. customThe residue is partitioned between ethyl acetate and water
4. concentrationThe organic phase is concentrated in vacuo
5. customto afford an amber solid residue
6. customis purified by flash chromatography (silica; ethyl acetate/hexanes)
7. customrecrystallized from methanol