反应详情

温度

70 °C

To a solution of N-(3 Methoxyphenylsulfonyl)D-tert-leucine benzyl ester (1.31 g, 3.35 mmol) in DMF (10 ml) is added K2CO3 (1.87 g, 13.4 mmol) followed by 1-iodo-3-methyl butane (1.33 g, 6.69 mmol) and the reaction mixture is heated to 70° C. overnight. The reaction is cooled to room temperature and then poured over 1 N HCl and extracted with Ethyl Acetate. The organics are washed with brine, dried over MgSO4 and concentrated. The crude product is purified by column chromatography eluting with a gradient of 5-40% (Hex-EtOAc) affording the title compound as a colorless oil (1.0 g, 65% yield). Mass spectrum (462.3; M+1).

1. temperatureThe reaction is cooled to room temperature
2. extractionextracted with Ethyl Acetate
3. washThe organics are washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe crude product is purified by column chromatography
7. washeluting with a gradient of 5-40% (Hex-EtOAc)