반응 #45858

반응 방정식

2-cyclopropyl-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile

N-bromosuccinimide

2,2′-azobis(isobutyronitrile)

→

compound

수율 82.0%

5-Bromomethyl-2-cyclopropyl-7-fluoro-6-phenyl-1,3-benzoxazole-4-carbonitrile

수율 82.0%

용매

carbon tetrachloride

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   기타the solvent was evaporated away under reduced pressure
3. 3
   기타the resulting residue was purified by middle-pressure liquid chromatography (eluent, n-hexane

실험 절차

Under nitrogen atmosphere, a carbon tetrachloride (12 ml) solution of 2-cyclopropyl-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-173) (1.00 g, 3.42 mmol), N-bromosuccinimide (913 mg, 5.13 mmol) and 2,2′-azobis(isobutyronitrile) (56 mg, 342 μmol) was stirred at 80° C. for 13 hours. After cooling, the solvent was evaporated away under reduced pressure, and the resulting residue was purified by middle-pressure liquid chromatography (eluent, n-hexane:ethyl acetate=5:1, v/v) to obtain the entitled compound (1.04 g, 82%) as a white solid.

출처