2-Methyl-1,3-cyclohexanedione synthesis
- Product Name:2-Methyl-1,3-cyclohexanedione
- CAS Number:1193-55-1
- Molecular formula:C7H10O2
- Molecular Weight:126.15
504-02-9
553 suppliers
$5.00/10g
1193-55-1
219 suppliers
$6.00/1g
Yield:1193-55-1 87%
Reaction Conditions:
with hydrogenchloride;formaldehyd;dimethyl amine;palladium-carbon in methanol;water;
Steps:
1 EXAMPLE 1
EXAMPLE 1 In a reactor equipped with a stirrer, 300 parts of methanol, 56 parts of 50% aqueous solution of dimethylamine and 56 parts of 1,3-cyclohexanedione were placed and the temperature of the mixture was raised to 30° C. Thereafter, 53 parts of 37% aqueous solution of formaldehyde was added dropwise for an hour. After adding, the reaction solution was maintained at 40° C. for 3 hours. The end of the reaction was confirmed by checking the amount of the remaining unreacted material (1,3-cyclohexanedione) by a high performance liquid chromatography. Then, 10 parts of 5% palladium-carbon was added to the resulting reaction mixture and hydrogen was blown over 15 hours at 30° C. under normal pressure. The end of the reaction was confirmed by checking the amount of the remaining unreacted material (2-dimethylaminomethyl-1,3-cyclohexanedione). After completion of the reaction, the catalyst was removed by filtration at 30° C. and 300 parts of water was added to the reaction mixture and methanol was removed by distillation, after which the residue was adjusted to pH 6 by adding 35% hydrochloric acid. The resulting precipitate was separated by filtration, washed with water, and was dried at 70° C. to obtain 54.8 parts of a dry cake of 2-methyl-1,3-cyclohexanedione (yield: 87.0%). The composition analysis of the dry cake by a high performance liquid chromatography revealed that the purity of 2-methyl-1,3-cyclohexanedione was 97.2%. The melting point of the dry cake was 206°-208° C. (the value described in literature: 207°-209° C.). The FD-mass spectrum of the dry cake had a peak at 126 and the value was the same as the theoretical molecular weight.
References:
US5276198,1994,A
608-25-3
441 suppliers
$10.00/5g
1193-55-1
219 suppliers
$6.00/1g
