反应详情

In a 10 ml glass tube were placed (5-phenyl-4-[(pyridin-2-ylmethyl)amino]thieno[2,3-d]pyrimidin-2-yl}acetic acid ethyl ester (35 mg, 0.088 mmol) and a saturated solution of methylamine in ethanol (2.0 ml). The tube was sealed with a septum and placed in the microwave cavity. Microwave irradiation of 200 W was used, the temperature being ramped from room temperature to 100° C. Once 100° C. was reached, the reaction mixture was held at this temperature for 30 minutes. The temperature was then ramped up to 150° C. and the reaction mixture was held at this temperature for a further 30 minutes. The resultant mixture was diluted with water (50 ml) and extracted with dichloromethane (3×50 ml). The combined organic extracts were dried (MgSO4) and the solvent removed in vacuo to give a residue which was purified by flash chromatography (silica) eluting with 5% methanol in dichloromethane to give N-methyl-2-{5-phenyl-4-[{pyridin-2-ylmethyl)amino]thieno[2,3-d]pyrimidin-2-yl}acetamide (2 mg).

1. customIn a 10 ml glass tube were placed
2. customThe tube was sealed with a septum
3. customMicrowave irradiation of 200 W
4. custombeing ramped from room temperature to 100° C
5. customOnce 100° C.
6. customwas then ramped up to 150° C.
7. waitthe reaction mixture was held at this temperature for a further 30 minutes
8. extractionextracted with dichloromethane (3×50 ml)
9. dry with materialThe combined organic extracts were dried (MgSO4)
10. customthe solvent removed in vacuo
11. customto give a residue which
12. customwas purified by flash chromatography (silica)
13. washeluting with 5% methanol in dichloromethane