反应详情

To a solution of (3RS,4SR)-1-benzyl-4-(3,4-dichloro-phenyl)-pyrrolidine-3-carboxylic acid methoxy-methyl-amide (3A) 6.58 g (0.017 mol) dissolved in THF (100 mL) was added 16 mL (0.017 mol) of lithiumaluminiumhydride (1.0M in THF) dropwise at 0° C. and stirred for one hour. The reaction was quenched by aq. ammonium chloride solution and extracted with ethylacetate twice. The combined organic layers were dried on anhydrous sodium sulfate and concentrated in vaccuo. The residue was purified by silica gel column chromatography eluted by a mixture of heptane and ethyl acetate (3:2) yielding 5.21 g (93%) of the title compound as a light yellow oil. ES-MS m/e: 334.2 (M+H+).

1. customThe reaction was quenched by aq. ammonium chloride solution
2. extractionextracted with ethylacetate twice
3. dry with materialThe combined organic layers were dried on anhydrous sodium sulfate
4. concentrationconcentrated in vaccuo
5. customThe residue was purified by silica gel column chromatography
6. washeluted by a mixture of heptane and ethyl acetate (3:2)