HRID258478

反应详情

EQUATION

反应方程式

HRID 258478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the lactone of Step 4 (1.004 g, 2.335 mmol) in 5 mL of anhydrous THF at r.t., a suspension of 0.70M 1,4-di(bromomagnesio)butane in THF (J. Org. Chem., 45, 1828 (1980); 5.3 mL, 3.7 mmol) was added dropwise and the mixture was stirred for 30 min and was quenched at 0° C. with cold 25% aq NH4OAc. The title cyclopentanol was extracted with EtOAc, dried over Na2SO4 and purified by flash chromatography on silica using EtOAc:toluene 15:85 and 20:80. Yield: 1.006 g, 88%.

WORKUP

后处理

  1. additionwas added dropwise
  2. customwas quenched at 0° C. with cold 25% aq NH4OAc
  3. extractionThe title cyclopentanol was extracted with EtOAc
  4. dry with materialdried over Na2SO4
  5. custompurified by flash chromatography on silica