反应详情

A mixture of 49 parts of iodomethane, 10.5 parts of 1-(2-chloroethyl)-1,4-dihydro-5H-tetrazol-5-one, 15 parts of sodium carbonate, 0.2 parts of potassium iodide and 240 parts of 4-methyl-2-pentanone is stirred and refluxed overnight with water-separator. The reaction mixture is cooled, 100 parts of water are added and the layers are separated. The aqueous phase is extracted with dichloromethane. The combined organic phases are dried, filtered and evaporated. The residue is purified by column-chromatography over silica gel using trichloromethane as eluent. The pure fractions are collected and the eluent is evaporated, yielding 15 parts (85%) of 1,4-dihydro-1-(2-iodoethyl)-4-methyl-5H-tetrazol-5-one as a residue.

1. temperatureThe reaction mixture is cooled
2. customthe layers are separated
3. extractionThe aqueous phase is extracted with dichloromethane
4. customThe combined organic phases are dried
5. filtrationfiltered
6. customevaporated
7. customThe residue is purified by column-chromatography over silica gel
8. customThe pure fractions are collected
9. customthe eluent is evaporated