반응 #8229

반응 방정식

methyl 4-[({2-[(4-bromobenzyl)oxy]phenethyl}amino)-methyl]benzoate

ethyl 5-bromovalerate

sodium bicarbonate

water

→

Methyl 4-{[{2-[(4-bromobenzyl)oxy]phenethyl}(5-ethoxy-5-oxopentyl)amino]methyl}benzoate

용매

acetonitrile

반응 조건

후처리

1. 1
   온도at reflux for 18 hours
2. 2
   추출extracted with methylene chloride
3. 3
   세척The organic phase is washed with saturated sodium chloride solution
4. 4
   건조dried over magnesium sulphate
5. 5
   workup.DISTILLATIONthe solvent is distilled off under reduced pressure
6. 6
   기타The residue is purified by chromatography over silica gel using the mobile phase methylene chloride/methanol 100/1

실험 절차

5.00 g (11.0 mmol) of methyl 4-[({2-[(4-bromobenzyl)oxy]phenethyl}amino)-methyl]benzoate from Ex. VIII, 2.30 g (11.0 mmol) of ethyl 5-bromovalerate and 1.109 g (13.21 mmol) of sodium bicarbonate in 30 ml of acetonitrile are heated at reflux for 18 hours. The reaction mixture is admixed with water and extracted with methylene chloride. The organic phase is washed with saturated sodium chloride solution and dried over magnesium sulphate and the solvent is distilled off under reduced pressure. The residue is purified by chromatography over silica gel using the mobile phase methylene chloride/methanol 100/1.

출처