反応 #2348087

反応方程式

ammonium chloride

methyl iodide

magnesium

3,4-difluorobromobenzene

→

2,3-difluorotoluene

溶媒

THF

tetrahydrofuran

反応条件

後処理

1. 1
   workup.ADDITIONthe dropwise addition
2. 2
   温度the mixture was refluxed for 1 hour
3. 3
   workup.ADDITIONadded
4. 4
   温度under cooling with an ice bath
5. 5
   その他to terminate
6. 6
   その他the reaction
7. 7
   抽出The aqueous layer was extracted with diethyl ether, which
8. 8
   workup.ADDITIONwas added to the organic layer
9. 9
   洗浄the organic layer was washed with a saturated saline
10. 10
    乾燥dried over anhydrous magnesium sulfate
11. 11
    workup.DISTILLATIONThe organic layer was distilled

実験手順

Under a nitrogen atmosphere, 82.5 g of 3,4-difluorobromobenzene (1) dissolved in 150 mL of tetrahydrofuran (THF) was added dropwise to 12.5 g of dried magnesium, and after completing the dropwise addition, the mixture was refluxed for 1 hour. The resulting solution was added dropwise to 15 mL of THF having 91.5 g of methyl iodide and 12.3 g of copper(I) iodide added thereto under cooling with an ice bath. After stirring over night, a saturated ammonium chloride aqueous solution was added thereto to terminate the reaction. The aqueous layer was extracted with diethyl ether, which was added to the organic layer, and the organic layer was washed with a saturated saline and then dried over anhydrous magnesium sulfate. The organic layer was distilled to obtain 37.6 g of 2,3-difluorotoluene (2)

出典