反应详情

1.35 g (34 mmol, 60%) sodium hydride are added to a solution of 4.87 g (28 mmol) of 5-methyl-3-p-tolyl-[1,2,4]triazole in 40 mL DMPU at 0° C. The reaction mixture is heated to ambient temperature and then stirred for one hour. 9.35 g (42 mmol) of tert.butyl (3-chloro-1,1-dimethyl-propyl)-carbamate and 1.87 g (5 mmol) of tetrabutylammonium iodide are added and the mixture is stirred overnight at ambient temperature and then for 2 hours at 80° C. It is combined with water and ethyl acetate, the aqueous phase is separated off and extracted with ethyl acetate. The combined organic phases are washed with water and sodium chloride solution, dried with sodium sulphate and evaporated down. The residue is purified by column chromatography (silica gel; petroleum ether/ethyl acetate=1.1). Oil.

1. stirringthe mixture is stirred overnight at ambient temperature
2. waitfor 2 hours at 80° C
3. customthe aqueous phase is separated off
4. extractionextracted with ethyl acetate
5. washThe combined organic phases are washed with water and sodium chloride solution
6. dry with materialdried with sodium sulphate
7. customevaporated down
8. customThe residue is purified by column chromatography (silica gel; petroleum ether/ethyl acetate=1.1)