HRID1864699

反应详情

EQUATION

反应方程式

HRID 1864699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of compound 4A (4.30 g, 12.0 mmol) in THF (75 mL) at −78° C. under nitrogen was added dropwise a solution of 1.0 M lithium triethylborohydride in tetrahydrofuran (60.0 mL, 60.0 mmol). The reaction was allowed to warm to rt and was stirred for 4 h. The reaction was then quenched by pouring over ice (150 g) and stirring for 30 min. The product was extracted into EtOAc and was washed with saturated aqueous NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated. Purification via flash chromatography (silica gel, 0-15% EtOAc in hexane) provided compound 5A (3.30 g).

WORKUP

后处理

  1. customThe reaction was then quenched
  2. additionby pouring over ice (150 g)
  3. stirringstirring for 30 min
  4. extractionThe product was extracted into EtOAc
  5. washwas washed with saturated aqueous NaHCO3
  6. dry with materialThe organic layer was dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customPurification via flash chromatography (silica gel, 0-15% EtOAc in hexane)