反应 #2348098

反应方程式

compound ( 10 )

2,3-difluoro-4-ethoxy-6-methylphenylboric acid

hydrogen peroxide

sodium

→

2,3-difluoro-5-methylphenol

溶剂

THF

反应条件

后处理

1. 1
   温度Under cooling with an ice bath
2. 2
   温度Under cooling with an ice bath
3. 3
   其他to terminate
4. 4
   其他the reaction
5. 5
   萃取an aqueous layer was extracted with diethyl ether, which
6. 6
   workup.ADDITIONwas added to the organic layer
7. 7
   洗涤The organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline
8. 8
   干燥dried over anhydrous magnesium sulfate
9. 9
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure

实验过程

Under cooling with an ice bath, 6.57 g of aqueous hydrogen peroxide was slowly added dropwise to the compound (10) having been dissolved in 37 mL of THF, followed by stirring at room temperature for 3 hours. Under cooling with an ice bath, 20 mL of a saturated sodium hydrogensufite aqueous solution was added thereto to terminate the reaction, and an aqueous layer was extracted with diethyl ether, which was added to the organic layer. The organic layer was washed with a saturated sodium hydrogensufite aqueous solution and saturated saline, and then dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 3.84 g of 2,3-difluoro-5-methylphenol (11).

来源