تفاعل #44713

معادلة التفاعل

N-{4-[(3-amino-1,2-benzisoxazol-4-yl)oxy]-3-fluorophenyl}-N-(2-amino-6-chloro-4-pyrimidinyl)amine

N-{4-[(3-Amino-1,2-benzisoxazol-4-yl)oxy]-3-fluorophenyl}-N-(2-amino-6-chloro-4-pyrimidinyl)amine

(4aR,7aR)-octahydro-6H-pyrrolo[3,4-b]pyridine

diisopropylethylamine

→

4-[(4aR,7aR)-Octahydro-6H-pyrrolo[3,4-b]pyridin-6-yl]-6-({4-[(3-amino-1,2-benz-isoxazol-4-yl)oxy]-3-fluorophenyl}amino)-2-pyrimidinylamine

المذيبات

2-ethylhexanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   ترشيحthe reaction mixture is filtered
3. 3
   workup.ADDITIONwater is added
4. 4
   استخلاصThe mixture is extracted repeatedly with ethyl acetate
5. 5
   تجفيفthe organic phase is dried over magnesium sulfate
6. 6
   أخرىthe solvent is removed under reduced pressure
7. 7
   أخرىThe residue is purified by preparative HPLC

الإجراء التجريبي

88 mg (0.23 mmol) of N-{4-[(3-amino-1,2-benzisoxazol-4-yl)oxy]-3-fluorophenyl}-N-(2-amino-6-chloro-4-pyrimidinyl)amine (from example 3) and 114.8 mg (0.91 mmol) of [(4aR,7aR)-octahydro-6H-pyrrolo[3,4-b]pyridine together with 294.1 mg (2.28 mmol) of diisopropylethylamine are dissolved in 4 ml of 2-ethylhexanol, and the mixture is stirred at 150° C. for 3 h. After cooling, the reaction mixture is filtered and water is added. The mixture is extracted repeatedly with ethyl acetate, the organic phase is dried over magnesium sulfate and the solvent is removed under reduced pressure. The residue is purified by preparative HPLC.

المصدر