反应详情

温度

0 °C

HATU (0.105 g, 0.28 mmol) was added into a mixture of 5-methyl-4-(2-(tetrahydro-2H-pyran-4-yloxy)pyridin-3-ylamino)thieno[2,3-d]pyrimidine-6-carboxylic acid (0.097 g, 0.25 mmol) and Hünig's base (44 μL, 0.25 mmol) in DMF (2.0 mL) at 0° C. The reaction mixture was stirred at 0° C. for 0.5 hours. 1-(2-Aminoethyl)-pyrrolidine (157 μL, 1.25 mmol) was added and the coolant removed. The reaction mixture was stirred at ambient temperature overnight. The solvent was concentrated in vacuo, the crude material added into water (10 mL) and the aqueous layer extracted into DCM. The product was purified by flash-column chromatography (DCM→10% ammonia/MeOH/DCM) to yield the title compound as off-white solid (0.051 g, 42% yield).

1. customthe coolant removed
2. stirringThe reaction mixture was stirred at ambient temperature overnight
3. concentrationThe solvent was concentrated in vacuo
4. additionthe crude material added into water (10 mL)
5. extractionthe aqueous layer extracted into DCM
6. customThe product was purified by flash-column chromatography (DCM→10% ammonia/MeOH/DCM)