反应详情

温度

110 °C

A mixture of 4-(4-methylpiperazin-1-yl)pyridin-3-amine (prepared according to methods similar to the one depicted in Preparation N-1, described below) (588.1 mg, 3.059 mmol), 2-amino-6-fluoro-pyrazolo[1,5-a]pyrimidine-3-carboxylic acid 5a (prepared according to methods similar to the ones depicted in the sequence Step 1-Step 2 of Preparation 2a) (500 mg, 2.549 mmol), TBTU (1.146 g, 3.569 mmol) and Et3N (515.9 mg, 710.6 μL, 5.098 mmol) in NMP (7 mL) was stirred at 110° C. in a sealed tube, for 20 h. The reaction mixture was diluted with EtOAc, washed with a saturated bicarbonate aqueous solution and brine. The organic was dried over MgSO4 and concentrated after filtration. The solid was triturated in DCM and then filtered off. It was further purified by Fractionlynx HPLC to yield the title compound as a colourless solid. MS (ES+) 371.3.

1. customprepared
2. customdepicted in Preparation N-1
3. customprepared
4. washwashed with a saturated bicarbonate aqueous solution and brine
5. dry with materialThe organic was dried over MgSO4
6. concentrationconcentrated
7. filtrationafter filtration
8. customThe solid was triturated in DCM
9. filtrationfiltered off
10. customIt was further purified by Fractionlynx HPLC