تفاعل #2254245

معادلة التفاعل

1,4-bis(3-aminopropyl)piperazine

4-fluorobenzaldehyde

water

→

1,4-bis{3-[N-(4-fluorobenzyl)amino]propyl}piperazine

المذيبات

ethanol

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGthe mixture was stirred for 12 h at room temperature
2. 2
   أخرىwas removed under reduced pressure
3. 3
   استخلاصThe aqueous residue was extracted with CH2Cl2 (3×30 mL)
4. 4
   استخلاصCombined organic layers were extracted with HCl 1M
5. 5
   استخلاصextracted with CH2Cl2
6. 6
   تجفيفCombined organic layers were dried over MgSO4
7. 7
   أخرىCrude compound is purified thick-layer chromatography (acetone/NH4OH:90/10)

الإجراء التجريبي

To a solution of 1,4-bis(3-aminopropyl)piperazine (0.51 mL, 2.5 mmol) and 4-fluorobenzaldehyde (0.59 mL, 5.5 mmol) in absolute ethanol (20 mL), 3 Å molecular sieves are added. After stirring the mixture at room temperature for 5 h, NaBH (0.47 g, 12.5 mmol) was added portionwise and the mixture was stirred for 12 h at room temperature. The reaction was quentched by dropwise addition of water (20 mL) and ethanol was removed under reduced pressure. The aqueous residue was extracted with CH2Cl2 (3×30 mL). Combined organic layers were extracted with HCl 1M. The combined aqueous layers were neutralized with NaOH 1M and extracted with CH2Cl2. Combined organic layers were dried over MgSO4. Crude compound is purified thick-layer chromatography (acetone/NH4OH:90/10).

المصدر