反应详情

温度

0 °C

To a three-necked, round bottom 5 L flask, equipped with a mechanical stirrer, gas inlet, thermometer and gas inlet, thermometer and gas outlet, was added 2,6-di-tert-butylphenol (474 g, 2.30 mole), ammonium thiocyanate (76.12 g, 4.83 mole) and methanol (1200 ml). The reaction mixture was stirred and cooled to 0° C. in an ice/salt bath. Maintaining the temperature at 0° to 10° C., chlorine gas was slowly bubbled through the mixture for about 1 hour whereupon the reaction mixture was a heterogeneous yellow color. Ammonia was then bubbled through the reaction for about 1-1/2 hours, maintaining the reaction mixture at a temperature of between 0° to 10° C. The reaction was stirred for an additional hour at 0° C., poured into 2 L of cold distilled water and refrigerated overnight. The aqueous phase was decanted and the solid taken up in methanol, precipitated from water, filtered and dried for 2 days over phosphorous pentoxide. The resulting gummy yellow solid was recrystallized from pentane and dried in vacuo to yield the product as a white powder, m.p. 61.5°-63° C.

1. customTo a three-necked, round bottom 5 L flask, equipped with a mechanical stirrer, gas inlet
2. temperatureMaintaining the temperature at 0° to 10° C.
3. customchlorine gas was slowly bubbled through the mixture for about 1 hour whereupon the reaction mixture
4. customAmmonia was then bubbled through the reaction for about 1-1/2 hours
5. temperaturemaintaining the reaction mixture at a temperature of between 0° to 10° C
6. stirringThe reaction was stirred for an additional hour at 0° C.
7. additionpoured into 2 L
8. distillationof cold distilled water and refrigerated overnight
9. customThe aqueous phase was decanted
10. customprecipitated from water
11. filtrationfiltered
12. dry with materialdried for 2 days over phosphorous pentoxide
13. customThe resulting gummy yellow solid was recrystallized from pentane
14. customdried in vacuo