تفاعل #58721

معادلة التفاعل

3-aminopyridine

Cs2CO3

compound 9

6-(3-methoxyphenyl)-2-(2-morpholin-4-yl-2-oxoethyl)pyrimidin-4-yl (trifluoromethyl)sulfonate

→

2-[6-(3-methoxyphenyl)-4-(3-pyridylamino)pyrimidin-2-yl]-1-morpholin-4-ylethan-1-one

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   أخرىA round bottom flask, oven dried
2. 2
   أخرىThe flask is purged with N2 for about 5-10 min
3. 3
   أخرىThe flask is equipped with a reflux condenser
4. 4
   أخرىpurged again with N2 for 5 min
5. 5
   درجة الحرارةthe reaction mixture is refluxed overnight
6. 6
   أخرىthe solvent is evaporated under reduced pressure
7. 7
   غسيلThe residue is washed with water (x2)
8. 8
   أخرىtriturated with methanol

الإجراء التجريبي

A round bottom flask, oven dried and kept under N2 atmosphere is charged with Cs2CO3 (1.4 eq), Pd(OAc)2 (5 mol %), and S-(−)-BINAP (7.5 mol %). The flask is purged with N2 for about 5-10 min and a solution of compound 9 (1 eq) in dry THF is added via a syringe, followed by 3-aminopyridine (2 eq) in one portion. The flask is equipped with a reflux condenser, purged again with N2 for 5 min and the reaction mixture is refluxed overnight. The reaction mixture is cooled down to room temperature and the solvent is evaporated under reduced pressure. The residue is washed with water (x2) and triturated with methanol to afford the desired 2-[6-(3-methoxyphenyl)-4-(3-pyridylamino)pyrimidin-2-yl]-1-morpholin-4-ylethan-1-one 10.

المصدر