反应详情

A solution of (S)-3-tert-Butoxycarbonylamino-4-methoxy-butyric acid benzyl ester (10.4 g, 32.3 mmol) in dry diethylether (70 ml) cooled to 0° C. is treated slowly with a 2.0 M solution of LiBH4 in THF (32.2 ml, 64.4 mmol). The reaction mixture is allowed to warm to ambient temperature and then left to stir. After 6 hours the reaction mixture is quenched slowly with 0.5 M aqueous solution of citric acid and extracted with ether. The ether phase is dried over magnesium sulphate and evaporated. The crude product is purified by flash silica chromatography (elution with a gradient 3:7 to 6:4 ethylacetate/hexane) to afford ((S)-3-Hydroxy-1-methoxymethyl-propyl)-carbamic acid tert-butyl ester as a clear oil. [M-BOC] 120.13

1. waitleft
2. customAfter 6 hours the reaction mixture is quenched slowly with 0.5 M aqueous solution of citric acid
3. extractionextracted with ether
4. dry with materialThe ether phase is dried over magnesium sulphate
5. customevaporated
6. customThe crude product is purified by flash silica chromatography (
7. washelution with a gradient 3:7 to 6:4 ethylacetate/hexane)