반응 #1863

반응 방정식

N-methyl-m-anisidine

triethylamine

toluene

2-bromopropionyl bromide

→

2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide

용매

Water

반응 조건

후처리

1. 1
   workup.ADDITIONwas added dropwise
2. 2
   기타the aqueous layer was collected
3. 3
   추출extracted with ethyl acetate
4. 4
   세척washed with 2N HCl
5. 5
   건조dried (Na2SO4)
6. 6
   기타The solvent was evaporated
7. 7
   기타to yield an oil which
8. 8
   기타was purified
9. 9
   workup.DISTILLATIONKugelrohr distillation
10. 10
    workup.DISSOLUTIONThe distillate was dissolved in isopropyl ether
11. 11
    기타The solid product, 2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide, m.p. 55°-56° C., crystallized from this solution

실험 절차

A solution of N-methyl-m-anisidine (265 g), triethylamine (269 ml) and toluene (550 ml) was stirred at 0° C. as 2-bromopropionyl bromide (202.6 ml) was added dropwise. The mixture was mechanically stirred overnight at room temperature. Water was added to the reaction and the aqueous layer was collected and extracted with ethyl acetate. All organic phases were combined, washed with 2N HCl, and dried (Na2SO4). The solvent was evaporated to yield an oil which was purified using Kugelrohr distillation. The distillate was dissolved in isopropyl ether. The solid product, 2-Bromo-N-(3-methoxyphenyl)-N-methyl-propanamide, m.p. 55°-56° C., crystallized from this solution.

출처