反应详情

温度

45 °C

30.0 g (0.232 mol) of 2,2,4-trimethyl-3-thiazoline and 17.6 g (0.255 mol) of sodium nitrite are dissolved in 75 ml of water and 26.6 ml (0.464 mol) of acetic acid are added dropwise, with stirring at 45° C. The internal temperature of the reaction mixture is allowed to rise slowly to 10°-15° C., and the mixture is then stirred at this temperature for an additional 2 hours. The product precipitates as ochre-brown crystals and is filtered, washed with water and dried in vacuo. A single recrystallization from chloroform/n-hexane yields 5-oxo-2,2,4-trimethyl-3-thiazoline oxime, m.p. 159°-161° C.

1. customto rise slowly to 10°-15° C.
2. stirringthe mixture is then stirred at this temperature for an additional 2 hours
3. customThe product precipitates as ochre-brown crystals
4. filtrationis filtered
5. washwashed with water
6. customdried in vacuo
7. customA single recrystallization from chloroform/n-hexane