HRID1162311

反应详情

EQUATION

反应方程式

HRID 1162311 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

tert-Butyl 1-(hydroxymethyl)-2-methoxy-2-methylpropylcarbamate (0.23 g) obtained in Example 73b) was dissolved in acetone (8 ml) and a 5% aqueous sodium hydrogen carbonate solution (2.7 ml). Potassium bromide (0.01 g), 2,2,6,6-tetramethyl-1-piperidinyloxy (0.17 g) and an aqueous sodium hypochlorite solution (1.7 ml) were added thereto, and mixed at 0° C. for 50 minutes. Acetone was distilled off under reduced pressure, and the residue was diluted with water, washed with diethyl ether, acidified with 1 N hydrochloric acid and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain the title compound as a pale yellow oil (0.20 g, 82%).

WORKUP

后处理

  1. additionmixed at 0° C. for 50 minutes
  2. distillationAcetone was distilled off under reduced pressure
  3. additionthe residue was diluted with water
  4. washwashed with diethyl ether
  5. extractionextracted with ethyl acetate
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. distillationthe solvent was distilled off under reduced pressure