HRID1514279

反应详情

EQUATION

反应方程式

HRID 1514279 的结构方程式

PROCEDURE

实验过程

A solution of 1,1-dimethylethyl 7-{5-[3-cyano-4-(methyloxy)phenyl]-1,2,4-oxadiazol-3-yl}-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (Preparation 54) (280 mg, 0.627 mmol) in hydrochloric acid 4M solution in dioxane (5 ml, 20.00 mmol) and 1,4-dioxane (5 ml) was stirred at room temperature overnight. The reaction mixture was filtered and washed with dioxane (˜5 ml), and the solid dried under vacuum to yield the title compound (177 mg, 0.393 mmol, 62.7% yield) as an off white solid. δH (d6DMSO, 400 MHz): 8.99-9.31 (2H, m), 8.53 (1H, s), 8.46 (1H, d), 7.96 (1H, s), 7.93 (1H, d), 7.54 (1H, d), 7.46 (1H, d), 4.07 (3H, s), 3.09-3.31 (7H, m); MS (ES): C20H18N4O2 requires 346; found 347 [M+H]+.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washwashed with dioxane (˜5 ml)
  3. customthe solid dried under vacuum