반응 #11327

반응 방정식

water

1,2,4-triazole

Sodium hydride

tritylchloride

→

1-trityl-1H-1,2,4-triazole

수율 47.0%

용매

DMF

hexane

DMF

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring for 1.5 hours at room temperature, to the reaction mixture
2. 2
   기타The precipitated crystal was collected by filteration
3. 3
   세척washed with water
4. 4
   workup.DISSOLUTIONdissolved in CHCl3 (800 ml)
5. 5
   기타dried
6. 6
   기타The solvent was evaporated
7. 7
   기타The obtained residue was chromatographed on silica gel (ethylacetate
8. 8
   농축The fraction of the objective was concentrated

실험 절차

Sodium hydride (60% dispersion in mineral oil, 13.8 g, 345 mmol) was washed with hexane and suspended in DMF (150 ml). At an ice bath temperature, 1,2,4-triazole (total; 20.7 g, 300 mmol) was added thereto in four divisions. After stirring for 30 minutes, to the mixture was added tritylchloride (total; 83.7 g, 300 mmol) in seven divisions and additionally added DMF (50 ml). After stirring for 1.5 hours at room temperature, to the reaction mixture was added water (600 ml). The precipitated crystal was collected by filteration, washed with water, dissolved in CHCl3 (800 ml) and dried. The solvent was evaporated. The obtained residue was chromatographed on silica gel (ethylacetate:CHCl3=1:2, v/v). The fraction of the objective was concentrated to give 1-trityl-1H-1,2,4-triazole (43.9 g). Yield: 47%.

출처