HRID1033895

反应详情

EQUATION

反应方程式

HRID 1033895 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

A solution of ethyl (E)-3-[2-n-butyl-1-{(2-chlorophenyl)methyl}-4-t-butyldimethylsilyloxymethyl-1H-imidazol-5-yl]-2-benzyl-2-propenoate (167 mg, 0.287 mmol) in absolute ethanol (3 mL) was treated portionwise at 6 hour intervals with 10% sodium hydroxide solution (3×1 mL). After being stirred overnight at 25° C., the reaction was heated to 50° C. for 4 hours, then concentrated in vacuo. The residual product was take0 up in water, acidified to pH 5-6 and extracted with methylene chloride. The isolated, dried, concentrated product was triturated with methanol/ether to provide 78 mg (62%) of the title compound; mp 176°-179° C. (d).

WORKUP

后处理

  1. temperaturethe reaction was heated to 50° C. for 4 hours
  2. concentrationconcentrated in vacuo
  3. extractionextracted with methylene chloride
  4. customThe isolated, dried
  5. customconcentrated product was triturated with methanol/ether