HRID722800

反应详情

EQUATION

反应方程式

HRID 722800 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

To a cold (0° C.) suspension of LiAlH4 (184 mg, 4.84 mmol) in THF (10 mL), a solution of ester 9 (375 mg, 0.97 mmol) in THF (2.5 mL) was added. The mixture was stirred at 0° C. for 2 h, and then quenched by dropwise addition of EtOH (3 ml). Na—K tartrate solution (10% aq, 30 mL) was added, and the crude was extracted with EtOAc (3×30 mL), dried over Na2SO4, concentrated in vacuo and purified by column chromatography on silica (hexane/EtOAc 5:1) to obtain alcohol 10 as a colorless oil (170 mg, 62% yield).

WORKUP

后处理

  1. customquenched by dropwise addition of EtOH (3 ml)
  2. additionNa—K tartrate solution (10% aq, 30 mL) was added
  3. extractionthe crude was extracted with EtOAc (3×30 mL)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. custompurified by column chromatography on silica (hexane/EtOAc 5:1)