反应详情

To a solution of 1-methyltetrazole-5-thiol sodium salt (2.00 g : 14.5 mMol.) in dimethylformamide (20 ml) under ice cooling is added bromochloromethane (20 ml) in one portion, and the mixture is stirred for 1.5 hour. The reaction mixture is diluted with water and extracted with ethyl acetate. The extract is washed with brine, dried over sodium sulfate, filtered, and concentrated. The residue is purified by silica gel column chromatography (toluene : ethyl acetate=20:1-10:1) to give 5-chloromethylthio-1-methyltetrazole as colorless crystals (1.73 g). Yield : 72%, m.p. 55° to 56° C.

1. extractionextracted with ethyl acetate
2. washThe extract is washed with brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue is purified by silica gel column chromatography (toluene : ethyl acetate=20:1-10:1)