2,6-dimethylheptan-4-one

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: As demonstrated by entries 4 and 5 in Table 1, at about 130° C., the conversion of the three-carbon feedstock starting from acetone and hydrogen is 16.4% and from isopropanol is 8.6%. Isopropanol becomes the major reaction product, while MIBC predominates over MIBK in the aldol product. Small amounts of mesityl oxide are also seen, however, no diisobutylketone is formed. Thus, 130° C. favors secondary alcohols over ketones and the conversion of three-carbon feedstock to aldol products is poor. As demonstrated by entries 4 and 5 in Table 1, at about 130° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: As demonstrated by entries 4 and 5 in Table 1, at about 130° C., the conversion of the three-carbon feedstock starting from acetone and hydrogen is 16.4% and from isopropanol is 8.6%. Isopropanol becomes the major reaction product, while MIBC predominates over MIBK in the aldol product. Small amounts of mesityl oxide are also seen, however, no diisobutylketone is formed. Thus, 130° C. favors secondary alcohols over ketones and the conversion of three-carbon feedstock to aldol products is poor. As demonstrated by entries 4 and 5 in Table 1, at about 130° C.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 10.00 g (79.3 mmol) 6-hydrazinopyrimidin-4-ol (CAS-No: 29939-37-5) were transformed in analogy to intermediate example 1c using 2,6-dimethylheptan-4-one to give after working up and purification 8.77 g (44%) of the title compound. to give purification 8.77 g (44%) of the title compound

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 10.00 g (79.3 mmol) 6-hydrazinopyrimidin-4-ol (CAS-No: 29939-37-5) were transformed in analogy to intermediate example 1c using 2,6-dimethylheptan-4-one to give after working up and purification 8.77 g (44%) of the title compound. to give purification 8.77 g (44%) of the title compound

Conditions: temp:35.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A stirred pressure reactor is charged with 183 ml of diisobutyl ketone. With stirring, 86.3 g of phenol (90%) are added. Then 103.8 g of 1,8-dichloroanthraquinone are added over 5 minutes and the reaction mixture is heated to boiling point. Distillation of water commences at 155° C. After 1.5 hours at this temperature, the reaction mixture is cooled to 35° C. and then 67 g of potassium carbonate are added. The batch is then heated to 160° C. over 90 minutes and allowed to react at this temperature for 1 hour. The reactor is then closed, heated to 175°-176° C. and kept at this temperature for 5 hours. After cooling to 30° C., the pressure in the reactor is reduced and the solvent is removed by distillation. To the reaction mixture are added 3 ml of 50% sodium hydroxide solution and the resultant 1,8-diphenoxyanthraquinone is isolated by filtration and vacuum dried, to give 141.0 g of a product with a titre of 86.2%, corresponding to a yield of 89.0%. The conversion is 99.9%. the reaction mixture is heated Distillation of water commences at 155° C 67 g of potassium carbonate are added The batch is then heated to 160° C. over 90 minutes to react at this temperature for 1 hour The reactor is then closed heated to 175°-176° C. kept at this temperature for 5 hours After cooling to 30° C. the solvent is removed by distillation To the reaction mixture are added 3 ml of 50% sodium hydroxide solution

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Optionally, the polyaminoamide-polyaminoimidazoline mixtures described above, which are to be used according to the present invention, can be reacted with common ketones such as acetone, methyl-ethyl ketone, di-ethyl ketone, methyl-isobutyl ketone, cyclohexanone, cyclopentanone, di-isobutyl ketone, 3,3,5-trimethyl cyclohexanone, or methyl-phenyl ketone, or with aldehydes such as acetaldehyde, butyraldehyde, isobutyraldehyde, or benzaldehyde to form the corresponding Schiff bases or enamines.

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Pd was found to be the most effective among metals used for the hydrogenation function of catalysts. The 1% wt. n-Pd/n-ZnCr2O4 gave the most active and selective catalyst for direct synthesis of MIBK from acetone. The highest MIBK selectivity of 72.1% was obtained at 77.3 wt % acetone conversion at 350° C. The total MIBK and DIBK selectivity of 85.6% was obtained at these conditions (Table 5, FIG. 2).

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Experiments 4, 5, 6, 7 and 8 were conducted in the same way as experiments 2 and 3. The details are stated in the table; the zinc particles had a largest dimension below 0.01 mm, see column 5. The diisobutyl ketone used in experiments 6 and 7 had a purity of 89 and 90%, respectively. At the end of experiments 4, 5, 6 and 7 the reaction mixture was free from dispersed zinc, see column 10, indicating that the zinc had been fully converted. The conversions of 2,3-dimethyl-2-butene and dichloroacetyl chloride are stated in columns 11 and 12, respectively. The yields of 2,2,3,3-tetramethylcyclopropanecarboxylic acid, presented in column 13, are slightly higher than that obtained in experiment 2. In the experiments 6 and 7 less brownish tarry material was formed than in the experiments 4 and 5 and the yield and purity of the TMCA formed were higher. The mixture obtained at the end of experiment 8 contained dispersed zinc and the yield of 2,2,3,3-tetramethylcyclopropanecarboxylic acid was only 49%, the molar ratio of zinc to dichloroacetyl chloride being 1.5.