反应详情

温度

-15 °C

To a solution of 1-carboxymethyl-1H-tetrazole-5-thiol (3.2 g) in dry acetone (60 ml) was added triethyl amine (4.2 g). After the addition of a solution of pivaloyl chloride (4.8 g) in dry acetone (10 ml) with stirring at -15° C. over a period of 5 minutes, the mixture was stirred for one hour and 15 minutes at the same temperature. A solution of 1-methylpiperazine (4.0 g) in dry acetone (10 ml) was dropwise added over a period of 5 minutes and the resulting mixture was stirred at -15° C. for 40 minutes and under ice-cooling for a further 2.5 hours. After the evaporation of the reaction mixture under reduced pressure, water was added to the residue, 4 N aqueous solution of sodium hydroxide was added until the crystals were dissolved. The resulting solution was evaporated under reduced pressure and the residue was crystallized from water to give 1-(4-methyl-1-piperazinyl) carbonylmethyl-1H-tetrazole-5 -thiol (2.2 g). mp>250° C.

1. stirringthe mixture was stirred for one hour and 15 minutes at the same temperature
2. stirringthe resulting mixture was stirred at -15° C. for 40 minutes and under ice-
3. temperaturecooling for a further 2.5 hours
4. customAfter the evaporation of the reaction mixture under reduced pressure, water
5. additionwas added to the residue, 4 N aqueous solution of sodium hydroxide
6. additionwas added until the crystals
7. dissolutionwere dissolved
8. customThe resulting solution was evaporated under reduced pressure
9. customthe residue was crystallized from water