HRID1605548

反应详情

EQUATION

反应方程式

HRID 1605548 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling
  2. filtrationthe precipitated sodium 3-benzyloxy-5-nitro-4-phenylbenzoate is collected by filtration
  3. washwashed with a small amount of icecold water
  4. customAfter drying
  5. dissolutionthe sodium salt is dissolved in hot water (100 ml)
  6. customthe 3-benzyloxy-5-nitro-4-phenylbenzoic acid is precipitated by addition of 4 N hydrochloric acid (10 ml)
  7. temperatureAfter cooling
  8. filtrationthe acid is collected by filtration
  9. washwashed with water
  10. customdried
  11. customAfter recrystallization twice from isopropanol
  12. customit is obtained with a melting point of 188.5°-189.5° C.