反应详情

温度

50 °C

A solution of N-benzyloxycarbonyl-L-glutamine methyl ester (25 g) in THF (500 ml) was added dropwise to a stirred solution of triphenylphosphine (44.5 g) in carbon tetrachloride (1 L). The mixture was heated to 50° C. for 2 hours. The mixture was evaporated. The resultant oil was triturated in ethyl acetate. The mixture was filtered and the filtrate was evaporated. The residue was purified by column chromatogaphy using a 1:1 mixture of hexane and ethyl acetate as eluant. There was thus obtained methyl (2S)-2-benzyloxycarbonylarnino-4-cyanobutyrate (19.38 g, 83%).

1. customThe mixture was evaporated
2. customThe resultant oil was triturated in ethyl acetate
3. filtrationThe mixture was filtered
4. customthe filtrate was evaporated
5. customThe residue was purified by column chromatogaphy
6. additiona 1:1 mixture of hexane and ethyl acetate as eluant