HRID471167

反应详情

EQUATION

反应方程式

HRID 471167 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of borane dimethylsulfide complex (2M in THF, 14.4 mL) was added dropwise to a solution of 2-(2,3-difluoro-4-hydroxyphenyl)acetic acid (example 77, step a) (1.08 g) in tetrahydrofuran (25 mL) at 0° C. and the resulting mixture was allowed to warm to RT and stirred overnight. The reaction was quenched with methanol and when bubbling had ceased the solvent evaporated. The residue was purified by silica gel chromatography eluting with 4:1 isohexane:ethyl acetate to ethyl acetate gradient. The fractions containing product were combined and evaporated to give the subtitled compound as white solid. Yield 0.95 g.

WORKUP

后处理

  1. customThe reaction was quenched with methanol and when
  2. custombubbling
  3. customevaporated
  4. customThe residue was purified by silica gel chromatography
  5. washeluting with 4:1 isohexane
  6. additionThe fractions containing product
  7. customevaporated