HRID1432048
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
- 0 °C
PROCEDURE
实验过程
Biphenyl-4-ol((5.26 g, 30.9 mmol), sodium iodide (4.635 g, 30.9 mmol), sodium hydroxide (1.276 g, 31.9 mmol) was dissolved in methanol (85 mL) and cooled to 0° C. To the solution was added 12% (w/v) sodium hypochlorite (20 mL) dropwise maintaining the temperature below 4° C. The solution was stirred at this temperature for 1 hour and then 2M sodium thiosulfite (50 mL) wad added and the pH of the solution was adjusted to >pH 7 with 1M HCl. The mixture was filtered and the filtrate was washed with water. The solid was dried in a vacuum oven and then the title product was obtained as crystals after recrystallisation from heptane. Yield 7.08 g, 77%.
WORKUP
后处理
- temperaturedropwise maintaining the temperature below 4° C
- filtrationThe mixture was filtered
- washthe filtrate was washed with water
- customThe solid was dried in a vacuum oven