反应详情

温度

60 °C

To a 4-neck flask with a gas inlet, condenser, thermometer, and addition funnel, 50 mL of deionized water and 31 g of sodium acetate was added and stirring was continued until the solid dissolved. At this point, 57 g of heptane, 20 g of toluene, and 30 g (0.146 moles) of 3,5-dichloro-4-ethyl-2-hydroxyaniline was added and the 2-phase mixture was warmed to 60° C. A solution of 53.2 g of 2-[2,4-bis(1,1-dimethylpropyl)phenoxy]butyryl chloride (0.157 moles, 8% excess) in 53 g of heptane was then added at 60° C.-65° C. The reaction was held for 2 hr at 60° C. -65° C., upon which time the area percent product by HPLC was 92% on a solvent-free basis. The two-phase mixture was heated to 75° C.-80° C. and held for 15 minutes. The agitator was stopped and the lower layer was decanted. The product solution was washed twice with 42 g of deionized water, cooled to 70° C. and seeded. The product slurry was cooled to 0° C.-5° C., and the product was collected by filtration, washed with cold heptane, and dried to give 66.9 g (90% yield), with an assay of 99.5% (wt.).

1. additionTo a 4-neck flask with a gas inlet, condenser, thermometer, and addition funnel
2. dissolutiondissolved
3. temperatureThe two-phase mixture was heated to 75° C.-80° C.
4. waitheld for 15 minutes
5. customthe lower layer was decanted
6. washThe product solution was washed twice with 42 g of deionized water
7. temperaturecooled to 70° C.
8. temperatureThe product slurry was cooled to 0° C.-5° C.
9. filtrationthe product was collected by filtration
10. washwashed with cold heptane
11. customdried
12. customto give 66.9 g (90% yield)