تفاعل #1863

معادلة التفاعل

N-methyl-m-anisidine

triethylamine

toluene

2-bromopropionyl bromide

→

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

المذيبات

Water

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر