反应详情

温度

55 °C

Into a three-necked, round-bottom flask fitted with a stirrer, thermometer, reflux condenser and dropping funnel was added 250 g of 96% 2-(2,4,6-trichlorophenoxy) ethanol, 250 ml carbon tetrachloride and 4 g of benzyl-trimethyl-ammonium chloride. The mixture was heated to 55° C. and 146 g thionyl chloride was added dropwise over 1.5 hours. After the addition of the thionyl chloride the temperature of the reaction was slowly raised to 80° C. for a total reaction tme of 2.5 to 3 hours. The end of the reaction was determined by GLC. The mixture was cooled to 60° C. and water slowly added to decompose the excess thionyl chloride. The phases were separated and the organic phase was washed with a 10% sodium hydroxide solution until it reached a pH of 7. After an additional separation of the phases the organic phase was washed again with water. After a further separation of phases, the carbon tetrachloride was distilled off to yield an oil which slowly crystallized to form 257 g of 2-(2,4,6-trichlorophenoxy)-ethyl chloride in a purity of 96%-98% and yield of 98%.

1. customInto a three-necked, round-bottom flask fitted with a stirrer
2. temperaturethermometer, reflux condenser
3. temperaturewas slowly raised to 80° C. for a total reaction tme of 2.5 to 3 hours
4. temperatureThe mixture was cooled to 60° C.
5. customThe phases were separated
6. washthe organic phase was washed with a 10% sodium hydroxide solution until it
7. customAfter an additional separation of the phases the organic phase
8. washwas washed again with water
9. customAfter a further separation of phases
10. distillationthe carbon tetrachloride was distilled off
11. customto yield an oil which
12. customslowly crystallized