تفاعل #2254238

معادلة التفاعل

Fmoc-1,2-diaminoethane

triethylamine

→

Fmoc amine

المذيبات

DMF

DMF

ظروف التفاعل

المعالجة

1. 1
   أخرىthe ice bath is removed
2. 2
   workup.STIRRINGstirring
3. 3
   أخرىis continued at room temperature
4. 4
   أخرى(RT)
5. 5
   أخرىfor 6 h
6. 6
   workup.ADDITIONThe reaction mixture is poured over 2 mL ice-cold water
7. 7
   أخرىpurified by preparative HPLC
8. 8
   تركيزAfter concentration and lyophilization

الإجراء التجريبي

To a solution of Fmoc-1,2-diaminoethane (0.06 mmol) in 0.4 mL DMF at 0° C., is added triethylamine (0.12 mmol) followed by dropwise addition of DOTA(OtBu)3 NHS ester (0.05 mmol) in 0.5 mL DMF for 10 min with stirring. After 10 min, the ice bath is removed and stirring is continued at room temperature (RT) for 6 h. The reaction mixture is poured over 2 mL ice-cold water and purified by preparative HPLC. After concentration and lyophilization, Fmoc amine monomer 23 is obtained which is further treated with 1 mL 20% piperidine in DMF, and the solution is stirred at RT for 30 min. The reaction mixture is poured over 2 mL ice-cold water and purified by preparative HPLC. After lyophilization, DOTA(OtBu)3-aminoethane 24 is obtained.

المصدر