HRID1944910

反应详情

EQUATION

反应方程式

HRID 1944910 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Solid LiAlH4 (29 mg, 0.713 mmol) was added to a stirring solution of Intermediate 86 (265 mg, 0.357 mmol) in THF (5 mL) at 0° C. After stirring for an hour H2O (0.029 mL), 15% (w/v) NaOH (0.029 mL), and H2O (0.087 mL) were added in order then stirred for additional 1 h. The resulting suspension was diluted with EtOAc (10 mL) and the organic layer was washed with H2O (15 mL), brine (15 mL), dried over Na2SO4, and concentrated to give crude alcohol (224 mg) as yellow solid. Chromatography (9:1, CH2Cl2/MeOH) afforded the title compound (110 mg, 43%) as yellow solid. ES/MS calcd. for C41H39N4O6S+ 715.3. Found m/z=715.4 (M+H)+.

WORKUP

后处理

  1. additionwere added in order
  2. washthe organic layer was washed with H2O (15 mL), brine (15 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated
  5. customto give crude alcohol (224 mg) as yellow solid