反应详情

To a solution of 6-benzyloxycarbonylamino-hexanoic acid (10 g, 38 mmol) in methanol (200 mL) at room temperature was added thionyl chloride (11 g, 95 mmol). The reaction mixture was then refluxed for 16 h. The solvent was concentrated in vacuo, the residue was dissolved in ethyl acetate (200 mL) and washed with brine (3×150 mL), dried over anhydrous magnesium sulfate, and concentrated in vacuo. The residue was purified by flash column chromatography (silica, 14% ethyl acetate in hexane) to afford the titled compound (6.2 g, 58%), a colorless liquid.

1. temperatureThe reaction mixture was then refluxed for 16 h
2. concentrationThe solvent was concentrated in vacuo
3. dissolutionthe residue was dissolved in ethyl acetate (200 mL)
4. washwashed with brine (3×150 mL)
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash column chromatography (silica, 14% ethyl acetate in hexane)