HRID21766

反应详情

EQUATION

反应方程式

HRID 21766 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A 21.56 g (86.55 mmol) sample of the compound from step 24a above was dissolved in 200 mL of THF, and the solution was cooled to 0° C. BH3 -dimethyl sulfide (86.5 mL, 2N) was added dropwise under a nitrogen atmosphere. The reaction was stirred at room temperature for 16 hr, then cooled to 0° C. and quenched by careful addition of 10% acetic acid in methanol. The mixture was reduced in volume on a rotary evaporator, and the concentrate was dissolved in ethyl acetate, which was washed successively with 1N HCl, water and sodium bicarbonate solution. The organic extract was dried over Na2SO4 and concentrated to afford the title product, 19.94 g (98% yield).

WORKUP

后处理

  1. temperaturecooled to 0° C.
  2. customquenched by careful addition of 10% acetic acid in methanol
  3. customThe mixture was reduced in volume on a rotary evaporator
  4. dissolutionthe concentrate was dissolved in ethyl acetate
  5. washwhich was washed successively with 1N HCl, water and sodium bicarbonate solution
  6. extractionThe organic extract
  7. dry with materialwas dried over Na2SO4
  8. concentrationconcentrated