HRID2079605

反应详情

EQUATION

反应方程式

HRID 2079605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

To a solution of [(4-chlorophenyl)-(3-methoxy-benzenesulfonyl)-amino]-acetic acid methyl ester (1.03 g, 2.7 mmol) in THF (20 mL) was added an aqueous solution (10 mL) of lithium hydroxide monohydrate (168 mg, 4.0 mmol) slowly under ice-cooled condition. The reaction mixture was stirred for 2 h at 25° C. THF was evaporated in vacuo and water was added. The mixture was washed with diethyl ether. The aqueous layer was acidified with 1(N) hydrochloride acid to pH 6, and extracted with ethyl acetate (3×20 mL). The combined organic layers were washed with water, dried (Na2SO4), and evaporated under reduced pressure to yield the title compound as pure solid compound, which used as such in the final coupling reaction. Yield: 810 mg (84%).

WORKUP

后处理

  1. temperaturecooled condition
  2. customTHF was evaporated in vacuo and water
  3. additionwas added
  4. washThe mixture was washed with diethyl ether
  5. extractionextracted with ethyl acetate (3×20 mL)
  6. washThe combined organic layers were washed with water
  7. dry with materialdried (Na2SO4)
  8. customevaporated under reduced pressure