2,4-二甲基-N-乙酰乙酰苯胺

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.48 kg/h (20.5 mol/h) of 2,4-dimethylaniline, 1.83 kg/h (21.3 mol/h) of diketene (purity 98%) and 8 kg/h of a mixture of 2.4 kg/h of ethanol and 5.6 kg/h of water are metered separately but simultaneously into a reactor which has been preheated to about 80° C. The reactor consists of a double-shell glass vessel of about 0.6 l capacity and is equipped with a stirrer, thermometer, reflux condenser and, at the bottom, with a run-off. Immediately the metering has started, the heat evolved by the reaction causes the reactor contents to reflux at about 85° C. The heating of the reactor is discontinued and the reaction is continued by limiting the reactor contents to about 0.3 1 by continuous pumping out. The reactor discharge is cooled to about 15° C. with stirring, and the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration. The moist product, which is obtained at about 5 kg/h, is washed with about 4 kg/h of cold aqueous 30% strength ethanol and dried, leaving 4 kg/h (19.5 mol/h) of 2',4'-dimethylacetoacetanilide (melting point about 89° C.) corresponding to a yield of 95% based on amine. are metered separately but simultaneously into a reactor has been preheated to about 80° C The reactor consists of a double-shell glass vessel of about 0.6 l capacity is equipped with a stirrer thermometer, reflux condenser The heating of the reactor The reactor discharge is cooled to about 15° C. the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration The moist product, which is obtained at about 5 kg/h is washed with about 4 kg/h of cold aqueous 30% strength ethanol dried

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.48 kg/h (20.5 mol/h) of 2,4-dimethylaniline, 1.83 kg/h (21.3 mol/h) of diketene (purity 98%) and 8 kg/h of a mixture of 2.4 kg/h of ethanol and 5.6 kg/h of water are metered separately but simultaneously into a reactor which has been preheated to about 80° C. The reactor consists of a double-shell glass vessel of about 0.6 l capacity and is equipped with a stirrer, thermometer, reflux condenser and, at the bottom, with a run-off. Immediately the metering has started, the heat evolved by the reaction causes the reactor contents to reflux at about 85° C. The heating of the reactor is discontinued and the reaction is continued by limiting the reactor contents to about 0.3 1 by continuous pumping out. The reactor discharge is cooled to about 15° C. with stirring, and the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration. The moist product, which is obtained at about 5 kg/h, is washed with about 4 kg/h of cold aqueous 30% strength ethanol and dried, leaving 4 kg/h (19.5 mol/h) of 2',4'-dimethylacetoacetanilide (melting point about 89° C.) corresponding to a yield of 95% based on amine. are metered separately but simultaneously into a reactor has been preheated to about 80° C The reactor consists of a double-shell glass vessel of about 0.6 l capacity is equipped with a stirrer thermometer, reflux condenser The heating of the reactor The reactor discharge is cooled to about 15° C. the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration The moist product, which is obtained at about 5 kg/h is washed with about 4 kg/h of cold aqueous 30% strength ethanol dried

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.48 kg/h (20.5 mol/h) of 2,4-dimethylaniline, 1.83 kg/h (21.3 mol/h) of diketene (purity 98%) and 8 kg/h of a mixture of 2.4 kg/h of ethanol and 5.6 kg/h of water are metered separately but simultaneously into a reactor which has been preheated to about 80° C. The reactor consists of a double-shell glass vessel of about 0.6 l capacity and is equipped with a stirrer, thermometer, reflux condenser and, at the bottom, with a run-off. Immediately the metering has started, the heat evolved by the reaction causes the reactor contents to reflux at about 85° C. The heating of the reactor is discontinued and the reaction is continued by limiting the reactor contents to about 0.3 1 by continuous pumping out. The reactor discharge is cooled to about 15° C. with stirring, and the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration. The moist product, which is obtained at about 5 kg/h, is washed with about 4 kg/h of cold aqueous 30% strength ethanol and dried, leaving 4 kg/h (19.5 mol/h) of 2',4'-dimethylacetoacetanilide (melting point about 89° C.) corresponding to a yield of 95% based on amine. are metered separately but simultaneously into a reactor has been preheated to about 80° C The reactor consists of a double-shell glass vessel of about 0.6 l capacity is equipped with a stirrer thermometer, reflux condenser The heating of the reactor The reactor discharge is cooled to about 15° C. the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration The moist product, which is obtained at about 5 kg/h is washed with about 4 kg/h of cold aqueous 30% strength ethanol dried

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: After the pressure drop (column 1: approx. 45 mbar, column 2: approx. 25 mbar) und the temperature profile (73-77° C.) had stabilized, m-xylidine (16.9 kg/h) was fed to the 2nd plate and diketene (total 12.0 kg/h) to plate Nos. 14, 15 and 16 of the first column. The diketene feed was started only after the xylidine-containing reflux had reached plate No. 14. und the temperature profile (73-77° C.) containing reflux

反应条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2.48 kg/h (20.5 mol/h) of 2,4-dimethylaniline, 1.83 kg/h (21.3 mol/h) of diketene (purity 98%) and 8 kg/h of a mixture of 2.4 kg/h of ethanol and 5.6 kg/h of water are metered separately but simultaneously into a reactor which has been preheated to about 80° C. The reactor consists of a double-shell glass vessel of about 0.6 l capacity and is equipped with a stirrer, thermometer, reflux condenser and, at the bottom, with a run-off. Immediately the metering has started, the heat evolved by the reaction causes the reactor contents to reflux at about 85° C. The heating of the reactor is discontinued and the reaction is continued by limiting the reactor contents to about 0.3 1 by continuous pumping out. The reactor discharge is cooled to about 15° C. with stirring, and the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration. The moist product, which is obtained at about 5 kg/h, is washed with about 4 kg/h of cold aqueous 30% strength ethanol and dried, leaving 4 kg/h (19.5 mol/h) of 2',4'-dimethylacetoacetanilide (melting point about 89° C.) corresponding to a yield of 95% based on amine. are metered separately but simultaneously into a reactor has been preheated to about 80° C The reactor consists of a double-shell glass vessel of about 0.6 l capacity is equipped with a stirrer thermometer, reflux condenser The heating of the reactor The reactor discharge is cooled to about 15° C. the light-colored crystals which are formed are separated from about 7 kg/h of the pale yellow mother liquor by filtration The moist product, which is obtained at about 5 kg/h is washed with about 4 kg/h of cold aqueous 30% strength ethanol dried