HRID1525667

反应详情

EQUATION

反应方程式

HRID 1525667 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl 4-{[(5-chloro-6-isopropoxypyridin-3-yl)oxy]methyl}-2,5-difluorobenzoate (Preparation 14, 400 mg, 1.03 mmol) in a mixture tetrahydrofuran/methanol (1/1 10 mL) was added an aqueous solution of sodium hydroxide (2M, 2.6 mL, 5.15 mmol). The reaction was stirred at room temperature for 2 hours and diluted with ethyl acetate (20 mL). An aqueous solution of hydrochloric acid (2M, 10 mL) was added to pH 1. The organic phase was extracted with ethyl acetate (2×10 mL) and the combined organic layers were washed with brine (20 mL), dried over magnesium sulfate, filtered and the solvent removed in vacuo to afford the title compound as a colourless oil (240 mg, 94% over two steps). No further purification undertaken.

WORKUP

后处理

  1. extractionThe organic phase was extracted with ethyl acetate (2×10 mL)
  2. washthe combined organic layers were washed with brine (20 mL)
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customthe solvent removed in vacuo