反应 #321737

反应方程式

water

4-cyano-4'-hydroxybiphenyl

acetic acid

sulphuric acid

water

→

4'-Hydroxybiphenyl-4-carboxylic Acid

反应条件

后处理

1. 1
   温度The mixture was heated
2. 2
   温度under reflux for 48 hours
3. 3
   其他the cooled reaction mixture
4. 4
   过滤the white precipitate filtered off
5. 5
   洗涤The aqueous filtrate was then washed with diethyl ether (4×70 ml)
6. 6
   洗涤the combined extracts were then washed with water (50 ml)
7. 7
   干燥dried (MgSO4)
8. 8
   过滤filtered
9. 9
   其他evaporated
10. 10
    其他to give a white solid
11. 11
    其他dried thoroughly
12. 12
    其他recrystallised (glacial acetic acid)
13. 13
    干燥dried in vacuo (P2O5, 0.30 mm Hg, 50° C., 5 hours)

实验过程

A mixture of concentrated sulphuric acid (115 ml) and water (115 ml) was added dropwise to a stirred suspension of 4-cyano-4'-hydroxybiphenyl 39 (25.62 g, 131.4 mmol) in glacial acetic acid (400 ml). The mixture was heated under reflux for 48 hours, the cooled reaction mixture was then poured into water (600 ml) with stirring and the white precipitate filtered off. The aqueous filtrate was then washed with diethyl ether (4×70 ml); the combined extracts were then washed with water (50 ml), dried (MgSO4) filtered and evaporated to give a white solid, both crops of product were combined, dried thoroughly and recrystallised (glacial acetic acid) and dried in vacuo (P2O5, 0.30 mm Hg, 50° C., 5 hours).

来源