HRID1722685

反应详情

EQUATION

反应方程式

HRID 1722685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3,3-Dimethylglutaric anhydride (455 mg, 3.2 mmol) in tetrahydrofuran (THF, 5 ml) was treated with sublimed potassium t-butoxide (395 mg, 3.5 mmol). After 30 min the solution was concentrated, poured into saturated NaHCO3 solution and washed with ether. The aqueous phase was acidified to pH 4 with 0.5 M H3PO4 and extracted with chloroform which was dried over Na2SO4 and evaporated to afford 179 mg (26%) of the desired product as an oil. NMR (300 MHz, CDCl3, ppm), 1.13 (s,6H), 1.47 (s,9H), 2.33 (s,2H), 2.45 (s,2H).

WORKUP

后处理

  1. concentrationAfter 30 min the solution was concentrated
  2. additionpoured into saturated NaHCO3 solution
  3. washwashed with ether
  4. extractionextracted with chloroform which
  5. dry with materialwas dried over Na2SO4
  6. customevaporated