Adipic Acid → HCID 131715119, compound

Participants

Reaction Conditions

Reaction Steps

The ester-alcohol can be obtained in the method of the present invention by not carrying out the alcohol removing ester-interchange reaction, or as an unreacted fraction in the ester-interchange reaction which distills between the bis compound and the starting diester. On the other hand, it can be obtained as an intermediate of direct alcohol removing ester-interchange reaction between the diester and the diol. Adipic acid 3-methyl-3-hydroxypropyl butyl ester (3-methyl-3-hydroxypropyl butyl adipate), an ester alcohol prepared from adipic acid, 1,3-butanediol, and butanol may be purified after dehydrating esterification as in Example 1, and catalyst removing treatment and then distillation. The boiling point is 155° to 160° C./0.2 mmHg. Using a mixture of 82.8 g of this product and 405 g of dibutyl adipate (mol ratio is 1:5.2) to which 0.5 g of butyl titanate was added, reaction was carried out under a reduced pressure of 20 mmHg and heating at 160° C. for 12 hours with stirring while removing 21.5 g (97%) of resulting butanol, and after completion of the reaction, catalyst removing alkali washing and water washing as well as distillation was carried out to obtain 342 g of DBA and 5.2 g of unreacted ester-alcohol and 94.9 g (75.8%) of 1,3-butanediol bis-butyl adipate having a boiling point of 235° to 245° C./0.8 mmHg and 7.6 g (8.4%) of a residual material which was considered to be an oligomer of n=2.

Provenance & Evidence