HRID55924

反应详情

EQUATION

反应方程式

HRID 55924 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled solution at 0° C. of 5-methoxy-1H-indole 3 (7.4 g, 50 mmol) in diethyl ether (150 ml) under nitrogen was added dropwise a solution of methylmagnesium bromide (3M) in diethyl ether (17.5 ml) and the mixture was stirred for 2 h at room temperature. The solution was then cooled at 0° C. and to this solution was added a solution of 1-naphthoylchloride (9.5 g, 50 mmol) in diethyl ether (100 ml) dropwise over a period of 15 min. After the addition was completed the solution was warmed up at room temperature and stirred for 2 h followed by slow addition of saturated ammonium chloride solution (375 ml) and stirred overnight. The white solid formed was filtered, washed by ether and dried under high vacuum to give 5-methoxy-3-(1-naphthoyl)-1H-indole 4 (11.3 g, 75%).

WORKUP

后处理

  1. temperatureThe solution was then cooled at 0° C. and to this solution
  2. additionAfter the addition
  3. temperaturewas warmed up at room temperature
  4. stirringstirred for 2 h
  5. stirringstirred overnight
  6. customThe white solid formed
  7. filtrationwas filtered
  8. washwashed by ether
  9. customdried under high vacuum