反应 #40266

反应方程式

N-chlorosuccinimide

6-bromo-2-naphthol

→

6-bromo-1-chloro-2-naphthol

收率 95.4%

溶剂

dichloromethane

反应条件

后处理

1. 1
   其他The synthesis of (S1-2)
2. 2
   温度The reaction solution was heated to room temperature
3. 3
   洗涤washed with saturated sodium bicarbonate solution and water
4. 4
   干燥dried over magnesium sulfate
5. 5
   workup.DISTILLATIONdistilled under a reduced pressure
6. 6
   其他to remove the solvent
7. 7
   其他Recrystallization

实验过程

The synthesis of (S1-2) was carried out following the method described in Synlett, No. 18, 2837 (2005), wherein 29.9 g of N-chlorosuccinimide and 600 ml of dichloromethane were added to a reactor in nitrogen atmosphere and cooled to 0° C., 2.6 g of zirconium (IV) chloride was added, and then 50 g of 6-bromo-2-naphthol (S1-1) was added slowly. The reaction solution was heated to room temperature and stirred for 10 hours, then washed with saturated sodium bicarbonate solution and water, dried over magnesium sulfate, and distilled under a reduced pressure to remove the solvent. Recrystallization was carried out using a mixed solvent of toluene/heptane=1/1 (volumetric ratio) to obtain 55 g of 6-bromo-1-chloro-2-naphthol (S1-2).

来源