HRID1646127

反应详情

EQUATION

反应方程式

HRID 1646127 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Lithium diisopropylamide (0.85 mmol, 1M in tetrahydrofuran) is cooled to -78° under argon and a solution of ethyl (E)-4-[2-n-butyl-1-[(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-3-(2-thienyl)methyl)-3-butenoate (0.709 mmol), prepared as in Example 13 using methyl (E) 3-[2-n-butyl-1-[(2-chlorophenyl)methyl]-1H-imidazol-5-yl]-(2-thienyl)methyl-2-propenoate (Example 1), in tetrahydrofuran (5 mL) is added. After 10 minutes methyl iodide (0.71 mmol) is added. The mixture is then stirred at room temperature overnight, diluted with 10% ammonium chloride and extracted with ethyl acetate. The dried, concentrated product is chromatographed over silica gel with 6:4 hexanes/ethyl acetate to give the title compound. (ii) (E)-1-[2-n-butyl-1-{(2-chlorophenyl)methyl}-1H-imidazol-5-yl]-3-methyl-3-(1H-tetrazol-5-yl)-2-(2-thienyl)methyl-1-propene

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. customThe dried, concentrated product is chromatographed over silica gel with 6:4 hexanes/ethyl acetate