HRID323006

反应详情

EQUATION

反应方程式

HRID 323006 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-78 °C

PROCEDURE

实验过程

A solution of 5-chloro-8-hydroxy-2-methylquinoline (9.2 g) in 55 mL of fluorosulfonic acid is stirred at 120° C. for 18 h in a tightly stoppered flask. The mixture is then cooled to −78° C. and poured onto an intimate mixture of 250 mL of crushed ice and 250 mL of powdered dry ice. The mixture is allowed to warm to 25° C., and then diluted with distilled water until further addition causes no additional solid to precipitate (ca. 100 mL). The mixture is filtered, and the solid obtained is washed with four 50 mL-portions of 0° C. distilled water and then dried in a stream of air to give 10.7 g of the title compound as an orange powder.

WORKUP

后处理

  1. temperatureto warm to 25° C.
  2. customto precipitate (ca. 100 mL)
  3. filtrationThe mixture is filtered
  4. customthe solid obtained
  5. washis washed with four 50 mL-portions of 0° C.
  6. distillationdistilled water
  7. customdried in a stream of air