反応 #55536

反応方程式

3-tert.butyl-5-methylthio-1,2,4-4H-triazole

phosgene

dimethyl amine

→

1-dimethylcarbamyl-3-tert.butyl-5-methylthio-1,2,4-1H-triazole

収率 87.0%

溶媒

toluene

toluene

反応条件

後処理

1. 1
   温度the reaction was heated
2. 2
   温度to reflux for 2 hrs
3. 3
   温度After cooling
4. 4
   洗浄the organic phase was washed with dilute hydrochloric acid
5. 5
   乾燥with water and was then dried over anhydrous sodium sulfate
6. 6
   その他The toluene was evaporated
7. 7
   その他the residue was crystallized from hexane
8. 8
   ろ過Filtration

実験手順

To a solution of 5.0 g (0.029 m) of 3-tert.butyl-5-methylthio-1,2,4-4H-triazole in toluene (100 ml) was added 50 ml of a toluene solution of phosgene (12%) and the reaction was heated to reflux for 2 hrs. After cooling, an excess of aqueous dimethyl amine was added and, after stirring at room temperature for 1 hr. the organic phase was washed with dilute hydrochloric acid, then with water and was then dried over anhydrous sodium sulfate. The toluene was evaporated to near dryness at reduced pressure and the residue was crystallized from hexane. Filtration gave 6.1 g (87%) of 1-dimethylcarbamyl-3-tert.butyl-5-methylthio-1,2,4-1H-triazole, MP 51°-53° C. Spectral properties agree with the structure as represented above:

出典