반응 #2348087

반응 방정식

ammonium chloride

methyl iodide

magnesium

3,4-difluorobromobenzene

→

2,3-difluorotoluene

용매

THF

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.ADDITIONthe dropwise addition
2. 2
   온도the mixture was refluxed for 1 hour
3. 3
   workup.ADDITIONadded
4. 4
   온도under cooling with an ice bath
5. 5
   기타to terminate
6. 6
   기타the reaction
7. 7
   추출The aqueous layer was extracted with diethyl ether, which
8. 8
   workup.ADDITIONwas added to the organic layer
9. 9
   세척the organic layer was washed with a saturated saline
10. 10
    건조dried over anhydrous magnesium sulfate
11. 11
    workup.DISTILLATIONThe organic layer was distilled

실험 절차

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)

출처