反应详情

温度

80 °C

In 100 ml of acetonitrile are dissolved 2.0 g of tert-butyl 3(R)-amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate and 3.0 g of ethyl 2-bromo-9-phthalimidononanoate, and 0.85 g of triethylamine is added to the solution. The mixture is heated at 80° C. for 3 days, concentrated under reduced pressure, diluted with 100 ml of water and extracted with 150 ml of ethyl acetate. The ethyl acetate layer is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The resulting oily substance is separated and purified by silicagel column chromatography (hexane:ethyl acetate=3:1-2:1) to give from the first fraction 0.9 g of tert-butyl 3(R)-[1(R)-ethoxycarbonyl-8-phthalimidooctyl]amino-4-oxo-2,3,4,5-tetrahydro-1,5-benzothiazepine-5-acetate as a colorless oil.

1. additionis added to the solution
2. concentrationconcentrated under reduced pressure
3. additiondiluted with 100 ml of water
4. extractionextracted with 150 ml of ethyl acetate
5. dry with materialThe ethyl acetate layer is dried over anhydrous magnesium sulfate
6. concentrationconcentrated under reduced pressure
7. customThe resulting oily substance is separated
8. custompurified by silicagel column chromatography (hexane:ethyl acetate=3:1-2:1)