HRID597557

反应详情

EQUATION

反应方程式

HRID 597557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a hot solution of 98.5 g. of 2'-benzoyl-2-bromo-acetanilide in 2 l methanol was added in one portion 39.0 g. of sodium azide. The mixture was heated to a slow reflux on a steam bath for 20 minutes. As the mixture cooled partially to room temperature, 18 ml. of benzyltrimethylammonium hydroxide (35% methanolic solution) was added. After standing overnight at room temperature, the orange-yellow needles that formed were collected, washed with methanol and dried at 60° C.; yield 76.6 g. (94%) of 3-azido-4-phenylcarbostyril, having a melting point of 120° - 140° dec. to high melting solid.

WORKUP

后处理

  1. temperatureThe mixture was heated to
  2. temperaturea slow reflux on a steam bath for 20 minutes
  3. customthe orange-yellow needles that formed
  4. customwere collected
  5. washwashed with methanol
  6. customdried at 60° C.