تفاعل #429684

معادلة التفاعل

benzyloxycarbonylpiperazine

triethylamine

3-dimethylaminopropyl chloride hydrochloride

triethylamine

→

brown viscous oil

المردود 103.5%

4-Benzyloxycarbonyl-3-dimethylaminopropylpiperazine

المردود 103.5%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 14 h
2. 2
   درجة الحرارةto reflux for 24 h
3. 3
   أخرىThe solvent was evaporated
4. 4
   استخلاصthe residue was extracted with ethyl actate
5. 5
   غسيلThe extract was washed with water
6. 6
   تجفيفdried (MgSO4)
7. 7
   تركيزconcentrated

الإجراء التجريبي

A suspension mixture of benzyloxycarbonylpiperazine (14.529, 65.9 mmol), 3-dimethyl-aminopropyl chloride hydrochloride (15.63 g, 98.9 mmol), and triethylamine (20.29, 200 mmol) in ethanol (100 ml) was refluxed for 14 h. Then 3-dimethylaminopropyl chloride hydrochloride (6.32 g, 40 mmol), and triethylamine (11.3 ml, 80 mmol) was added to the reaction mixture and continued to reflux for 24 h. The solvent was evaporated and the residue was extracted with ethyl actate. The extract was washed with water, dried (MgSO4), and concentrated to give 12.65 g of brown viscous oil, which was purified by column chromatography on silica gel (ammonium hydroxide aqueous solution/methanol/dichloromethane: 1/10/100) to give 2.21 g of brown clear oil.

المصدر