HRID1850001

反应详情

EQUATION

反应方程式

HRID 1850001 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-(4-chloro-phenoxy)-2-methyl-propionic acid ethyl ester (2.0 g, 8.24 mmol) in tetrahydrofuran (16 mL) at room temperature is added water (4 mL) followed by lithium hydroxide monohydrate (0.69 g, 16.4 mmol). The reaction is stirred for 16 h at room temperature. After this time, the mixture is diluted with water and washed with DCM. The aqueous phase is separated, acidified to pH ˜2 with 1M aqueous HCl solution and then extracted with DCM (x2). The combined organic extracts are washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure to give the title compound as a white solid (1.45 g, 82%). 1H NMR (400 MHz, CHLOROFORM-d): δ ppm 1.62 (6H, s), 6.89 (2H, d, J=9.0 Hz), 7.24 (2H, d, J=9.0 Hz).

WORKUP

后处理

  1. washwashed with DCM
  2. customThe aqueous phase is separated
  3. extractionextracted with DCM (x2)
  4. washThe combined organic extracts are washed with brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure