反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- filtrationthe precipitated pale yellow reaction product was filtered off with suction
- washwashed thoroughly several times with 50 cc each of water
- customdried in the air
- custom4.23 gm (42% of theory) of yellow crystals, m.p. 121°-122° C., were obtained (
- customafter twice recrystallizing from petroleum ether/ethyl acetate 1:1 using activated carbon) and