تفاعل #1473050

معادلة التفاعل

triethylamine

diethylcarbamoyl chloride

dimethylaminopyridine

3-(tetrahydropyran-2-yl)methylthio-1,2,4-triazole

3-(Tetrahydropyran-2-yl)methylthio-1,2,4-triazole

→

1-Diethylcarbamoyl-3-(tetrahydropyran-2-yl)methylthio-1,2,4-triazole

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةunder reflux for 2 hours
3. 3
   workup.DISTILLATIONThe solvent was distilled off
4. 4
   أخرىthe residue was purified by chromatography over silica gel
5. 5
   أخرى11.2 g (44% of theory) of a viscous clear oil were obtained

الإجراء التجريبي

11.6 g (85 mmol) of diethylcarbamoyl chloride and a spatula-tipful of dimethylaminopyridine were added to a solution of 200 ml of absolute tetrahydrofuran and 17.0 g (85 mmol) of 3-(tetrahydropyran-2-yl)methylthio-1,2,4-triazole (step b). 9.5 g (94 mmol) of triethylamine were then added dropwise and the mixture was heated under reflux for 2 hours. The solvent was distilled off and the residue was purified by chromatography over silica gel. 11.2 g (44% of theory) of a viscous clear oil were obtained. (1H-NMR (CDCl3; δ in ppm): 8.75 (s,1H); 4.00 (d,1H); 3.70-3.50 (bm,5H); 3.40 (dt,1H); 3.25 (d,2H); 1.85 (d,1H); 1.80 (d,1H); 1.65-1.45 (m,4H); 1.30 (t,6H))

المصدر