HRID1605548
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
PROCEDURE
实验过程
A mixture of 3-hydroxy-5-nitro-4-phenylbenzoic acid (3.0 g), benzylbromide (1.5 ml) and 1 N sodium hydroxide (30 ml) is stirred at room temperature for 6-7 hours. After cooling, the precipitated sodium 3-benzyloxy-5-nitro-4-phenylbenzoate is collected by filtration and washed with a small amount of icecold water. After drying, the sodium salt is dissolved in hot water (100 ml), and the 3-benzyloxy-5-nitro-4-phenylbenzoic acid is precipitated by addition of 4 N hydrochloric acid (10 ml). After cooling, the acid is collected by filtration, washed with water and dried. After recrystallization twice from isopropanol, it is obtained with a melting point of 188.5°-189.5° C.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe precipitated sodium 3-benzyloxy-5-nitro-4-phenylbenzoate is collected by filtration
- washwashed with a small amount of icecold water
- customAfter drying
- dissolutionthe sodium salt is dissolved in hot water (100 ml)
- customthe 3-benzyloxy-5-nitro-4-phenylbenzoic acid is precipitated by addition of 4 N hydrochloric acid (10 ml)
- temperatureAfter cooling
- filtrationthe acid is collected by filtration
- washwashed with water
- customdried
- customAfter recrystallization twice from isopropanol
- customit is obtained with a melting point of 188.5°-189.5° C.