HRID419759

反应详情

EQUATION

反应方程式

HRID 419759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

The 3-tert-butyl 4-methyl 2,2-dimethyloxazolidine-3,4-dicarboxylate (6.42 g, 24.97 mmol) obtained in the above-described reaction was dissolved in toluene (50 ml) and cooled to −78° C.; subsequently, a toluene solution of diisobutylaluminum hydride (0.93 M) was slowly added dropwise. After 30 minutes, methanol was added to the mixture and the reaction was stopped; a 10% potassium sodium tartrate solution (150 ml) was further added, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, filtered and concentrated. The resulting concentrate was purified by silica gel column chromatography to produce tert-butyl 4-formyl-2,2-dimethyloxazolidine-3-carboxylate (4.22 g, 74% yield).

WORKUP

后处理

  1. extractionthe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. concentrationThe resulting concentrate
  6. customwas purified by silica gel column chromatography