HRID1577546

反应详情

EQUATION

反应方程式

HRID 1577546 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 10.0 gm (0.0393 mol) of 2-benzoylbenzo[b]-thiophen-3-ol, 60 cc of concentrated aqueous ammonia and 250 cc of ethanol was heated for 20 hours at a temperature of 120° C. after introducing 5 bar of ammonia gas into the vessel. After cooling, the mixture was stirred into 1.5 liters of water, the precipitated pale yellow reaction product was filtered off with suction, washed thoroughly several times with 50 cc each of water and dried in the air. 4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (after twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and were found to be completely identical with the product obtained in Example 1 based on elemental analysis, IR and UV spectra.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationthe precipitated pale yellow reaction product was filtered off with suction
  3. washwashed thoroughly several times with 50 cc each of water
  4. customdried in the air
  5. custom4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (
  6. customafter twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and