HRID1689445

反应详情

EQUATION

反应方程式

HRID 1689445 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A solution of sodium hydroxide (1 g) in water (50 mL) was added to a solution of methyl 2-(2-fluorophenyl)-2-methylpropanoate (example 90, step b) (2.6 g) in methanol (50 mL) and THF (50 mL). The reaction mixture was heated at 40° C. for 40 hours. The organics were removed under reduced pressure and the remaining aqueous solution washed with ethyl acetate. The aqueous layer was cooled and acidified by addition of concentrated HCl. The mixture was extracted with ethyl acetate and the organic layer washed with brine before being dried over sodium sulphate, filtered and the solvent removed under reduced pressure to afford the subtitled compound. Yield 1.5 g.

WORKUP

后处理

  1. customThe organics were removed under reduced pressure
  2. washthe remaining aqueous solution washed with ethyl acetate
  3. temperatureThe aqueous layer was cooled
  4. additionacidified by addition of concentrated HCl
  5. extractionThe mixture was extracted with ethyl acetate
  6. washthe organic layer washed with brine
  7. dry with materialbefore being dried over sodium sulphate
  8. filtrationfiltered
  9. customthe solvent removed under reduced pressure