تفاعل #8229

معادلة التفاعل

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

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر