HRID471216

反应详情

EQUATION

反应方程式

HRID 471216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

Borane-methyl sulfide (2M in THF, 12.35 mL) was added dropwise to a solution of 2-(2-fluorophenyl)-2-methylpropanoic acid (example 90, step c) (1.5 g) in THF (30 mL). The reaction mixture was stirred at 20° C. for 8 hours. The mixture was quenched by careful addition of methanol until evolution of gas ceased. The solvents were removed under reduced pressure and the residue azeotroped with toluene. The crude product was purified by flash silica chromatography using 30% ethyl acetate in isohexane as solvent. Pure fractions were evaporated to dryness to afford the subtitled compound. Yield 1.3 g.

WORKUP

后处理

  1. customThe mixture was quenched by careful addition of methanol until evolution of gas
  2. customThe solvents were removed under reduced pressure
  3. customthe residue azeotroped with toluene
  4. customThe crude product was purified by flash silica chromatography
  5. customPure fractions were evaporated to dryness