反应详情

温度

120 °C

5-(Benzylthio)-7-chloro[1,3]thiazolo[4,5-d]pyrimidin-2-amine (6.0 g, 19.4 mmol) was dissolved in NMP (25 mL). DIPEA (6.8 mL, 38.8 mmol) and (2R)-2-(methylamino)pentan-1-ol (3.4 g, 29.1 mmol) were added and the mixture was heated to 120° C. for 3 days. Additional (2R)-2-(methylamino)pentan-1-ol (350 mg, 2.99 mmol) and DIPEA (1 mL, 5.74 mmol) was added and the reaction mixture was heated for 6 h at 120° C. After cooling to room temperature, the mixture was poured into ice. The precipitated product was collected by filtration and purified by flash column chromatography (eluent DCM:ethyl acetate gradient) to yield the title compound (5.74 g, 76% yield).

1. temperaturethe reaction mixture was heated for 6 h at 120° C
2. temperatureAfter cooling to room temperature
3. additionthe mixture was poured into ice
4. filtrationThe precipitated product was collected by filtration
5. custompurified by flash column chromatography (eluent DCM:ethyl acetate gradient)