反应详情

温度

85 °C

To 161.8 g. of methyl[(3,6-dichloro-2-methoxybenzoyl) aminooxy]acetate was added 80 g. of n-butyl alcohol, 600 ml. of toluene, and 9.5 g. of titanium n-butoxide. The mixture was stirred and heated to 85° C. for 2 hours to drive off a methanol/toluene mixture. The heat was then maintained at 95°-100° C. to distill off n-butanol/toluene. The reaction mixture was cooled to 40° C. and 150 ml. of 1 M. HCl added. The mixture was then washed with 1 M. HCl, water, then saturated NaHCO3 solution, and then dried over MgOS4, filtered, and evaporated in vacuo to yield the title product as a white solid, m.p. 68°-71° C.

1. temperatureThe heat was then maintained at 95°-100° C.
2. distillationto distill off n-butanol/toluene
3. temperatureThe reaction mixture was cooled to 40° C.
4. additionHCl added
5. washThe mixture was then washed with 1 M
6. dry with materialHCl, water, then saturated NaHCO3 solution, and then dried over MgOS4
7. filtrationfiltered
8. customevaporated in vacuo