HRID25689

反应详情

EQUATION

反应方程式

HRID 25689 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [1-(3,3-diethoxy-propylcarbamoyl)-2-hydroxy-3-methyl-butyl]-carbamic acid benzyl ester (350 mg, 0.854 mmol) in anhydrous tetrahydrofuran (2 ml) was added 0.5N hydrochloric acid (2 ml). The resulting solution was stirred for 20 minutes at room temperature. The aqueous layer was basified to pH 8 with sodium bicarbonate solution, and extracted with ethyl acetate (3×40 mL). The combined extracts were washed with saturated sodium chloride, dried over magnesium sulfate, filtered and concentrated in vacuo to provide [2-hydroxy-3-methyl-1-(3-oxo-propylcarbamoyl)-butyl]-carbamic acid benzyl ester (266 mg, 93%) as a white solid.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×40 mL)
  2. washThe combined extracts were washed with saturated sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo