反应详情

Ethyl 2-isocyanatopropanoate (104 mg, 0.73 mmol) was added to a suspension of N-(2-aminoethyl)-4-(5-(thiophen-2-yl)thiophen-2-yl)pyrimidin-2-amine (200 mg, 0.66 mmol) in dichloromethane (10 mL) at rt and stirred for 8 h. The solid was filtered off and added to 15 mL of hydrochloric acid (5 M). After refluxing for 6 h, the mixture was cooled to rt and the precipitate was filtered off, washed with water and then dissolved in 10 mL of methanol. 50 mg of potassium carbonate was added and the mixture was stirred for 10 min. 20 mL of dichloromethane was added and the mixture was filtered through Celite. The filtrate was concentrated to give the title compound (180 mg, 68%). MS (M+H)+ 400.

1. filtrationThe solid was filtered off
2. additionadded to 15 mL of hydrochloric acid (5 M)
3. temperatureAfter refluxing for 6 h
4. filtrationthe precipitate was filtered off
5. washwashed with water
6. dissolutiondissolved in 10 mL of methanol
7. addition50 mg of potassium carbonate was added
8. stirringthe mixture was stirred for 10 min
9. addition20 mL of dichloromethane was added
10. filtrationthe mixture was filtered through Celite
11. concentrationThe filtrate was concentrated