反应详情

81.1 To a solution of (3R,4S)-3-{[(5-chloro-thiophene-2-carbonyl)-amino]-methyl}-4-hydroxy-pyrrolidine-1-carboxylic acid tert-butyl ester (600 mg, prepared according to example 79.5) in 10 ml of CH2Cl2 was added at 5° C. 2.30 ml of NEt3 and 1.59 g of SO3-pyridine complex, the solution was warmed to 22° C. and stirring was continued for 3 h. The mixture was washed with aqueous NH4Cl, the organic layer was dried and evaporated. The residue was chromatographed on silica (heptane/AcOEt, 2:1) to give 435 mg of (R)-3-{[(5-chloro-thiophene-2-carbonyl)-amino]-methyl}-4-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester. Pale yellow solid. MS 303.0 ([M-isobutene+H]+)

1. washThe mixture was washed with aqueous NH4Cl
2. customthe organic layer was dried
3. customevaporated
4. customThe residue was chromatographed on silica (heptane/AcOEt, 2:1)