反应详情

A mixture of 3-chloro-5-ethynyl-2-methylthiopyridine (0.5 g, 2.72 mmol), 1-nitropropane (0.24 g, 0.27 mmol), 1,4-phenylenediisocyanate (1.3 g, 7.93 mmol) and triethylamine (5 drops) in benzene (20 mL) was heated under reflux with stirring for 8 hours, and allowed to stir at room temperature overnight. Water (1 mL) was added and the mixture stirred at room temperature for 2 hours. It was filtered through Celite, dried over anhydrous sodium sulphate and evaporated under reduced pressure. Recrystallisation of the residue from hexane gave the desired product (0.33 g, 48%) as a cream solid, melting point. 78-80° C.

1. temperaturewas heated
2. temperatureunder reflux
3. stirringto stir at room temperature overnight
4. stirringthe mixture stirred at room temperature for 2 hours
5. filtrationIt was filtered through Celite
6. dry with materialdried over anhydrous sodium sulphate
7. customevaporated under reduced pressure
8. customRecrystallisation of the residue from hexane