HRID574633

反应详情

EQUATION

反应方程式

HRID 574633 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

According to Scheme 2, step 1: To a solution of 4-Bromo-6-fluoro-indan-1-one (10.0 g, 43.7 mmol) in ethanol (183 ml) at 0° C. NaBH4 (3.67 g, 97.0 mmol) was added in portions and then the mixture was stirred at room temperature for 18 h. After evaporation of solvents in vacuo, water was added to the residue, the solution was extracted 3 times with ethyl acetate, then 2N aqueous HCl was added and the combined organic layers were washed with saturated aq. NaHCO3 and water. After drying over Na2SO4 and filtration, solvents were evaporated in vacuo to give 10.0 g of 4-Bromo-6-fluoro-indan-1-ol (4a) which was used immediately in the next step without purification.

WORKUP

后处理

  1. customat 0° C
  2. customAfter evaporation of solvents in vacuo, water
  3. additionwas added to the residue
  4. extractionthe solution was extracted 3 times with ethyl acetate
  5. addition2N aqueous HCl was added
  6. washthe combined organic layers were washed with saturated aq. NaHCO3 and water
  7. dry with materialAfter drying over Na2SO4 and filtration, solvents
  8. customwere evaporated in vacuo