反应详情

To a suspension of 1,2,3-triazol-4-thiol sodium salt (109 g : 870 mMol.) in dimethylformamide (300 ml) is added dropwise at -20° to -30° C. chloromethyl thiolacetate (109 g : 870 mMol.), and the mixture is stirred at room temperature for 2 hours. To the reaction mixture are added under ice cooling trityl chloride (292 g; 1.05 Mol.) and pyridine (84.6 ml : 1.05 Mol.), and the mixture is stirred at room temperature for 18 hours, diluted with dichloromethane, washed with brine, dried over sodium sulfate, and concentrated under reduced pressure. The residue is crystallized from ether to give 4-acetylthiomethylthio-1-trityl-1,2,3-triazole (183 g). Yield: 49%. mp. 115° to 116° C. Colorless crystals.

1. additionTo the reaction mixture are added under ice
2. stirringthe mixture is stirred at room temperature for 18 hours
3. washwashed with brine
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue is crystallized from ether