反応 #11327

反応方程式

water

1,2,4-triazole

Sodium hydride

tritylchloride

→

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

収率 47.0%

溶媒

DMF

hexane

DMF

反応条件

後処理

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

実験手順

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%.

出典