反应 #67990

反应方程式

tetrahydrofuran

m-anisidine

triethylamine

allyl bromide

→

N-allyl-3-methoxyaniline

溶剂

ethyl acetate

Water

反应条件

后处理

1. 1
   workup.ADDITIONwere added
2. 2
   温度under cooling with ice
3. 3
   其他The organic layer was separated
4. 4
   其他the aqueous layer was separated with ethyl acetate
5. 5
   洗涤the resultant solution was washed with an aqueous saturated sodium chloride solution
6. 6
   干燥dried over anhydrous magnesium sulfate
7. 7
   其他the solvent was removed under reduced pressure
8. 8
   其他The residue thus obtained
9. 9
   其他was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=5:1]

实验过程

To 10 mL of a tetrahydrofuran solution containing 1.0 g of m-anisidine, 1.2 mL of triethylamine and 0.70 mL of allyl bromide were added under cooling with ice. The reaction mixture was stirred for 30 minutes. Water and ethyl acetate were added thereto. The organic layer was separated, and the aqueous layer was separated with ethyl acetate. The organic layer and the extract were combined, the resultant solution was washed with an aqueous saturated sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=5:1] to obtain 0.36 g of a yellow oily substance, N-allyl-3-methoxyaniline.

来源