تفاعل #44735

معادلة التفاعل

ethyl acetate

6-chloro-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)-phenyl]pyrimidine-2,4-diamine

6-Chloro-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]pyrimidine-2,4-diamine

3-[(2,4-dimethoxybenzyl)amino]propan-1-ol

TFA

→

3-[(2-Amino-6-{[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)phenyl]amino}-pyrimidin-4-yl)amino]propan-1-ol

المذيبات

DCM

1-butanol

N-ethyl-diisopropylamine

ظروف التفاعل

المعالجة

1. 1
   أخرىVolatile components are removed under reduced pressure
2. 2
   أخرىthe residue is purified by preparative HPLC
3. 3
   أخرىThe substrate obtained
4. 4
   استخلاصextracted with sat. sodium carbonate solution
5. 5
   تجفيفThe organic phase is dried over sodium sulfate
6. 6
   أخرىthe solvent is removed under reduced pressure
7. 7
   أخرىThe residue is purified by preparative HPLC

الإجراء التجريبي

78 mg (0.21 mmol) of 6-chloro-N4-[3-fluoro-4-(1H-pyrrolo[2,3-b]pyridin-4-yloxy)-phenyl]pyrimidine-2,4-diamine (from example 60), 190 mg (0.84 mmol) of 3-[(2,4-dimethoxybenzyl)amino]propan-1-ol in 1 ml of 1-butanol and 0.37 ml of N-ethyl-diisopropylamine are, in a closed pressure vessel, heated at 130° C. overnight. Volatile components are removed under reduced pressure, and the residue is purified by preparative HPLC. The substrate obtained is taken up in 2 ml of DCM, and 0.5 ml of TFA is added. The mixture is stirred at RT for 20 min and then poured into ethyl acetate and extracted with sat. sodium carbonate solution. The organic phase is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC.

المصدر