Water → 3-Cyclohexene-1,2-dicarboxylic acid
Reaction equation
N1C(N)=NC(N)=NC=1N.[C:10]1(=[O:20])[O:15][C:13](=[O:14])[CH:12]2[CH2:16][CH2:17][CH:18]=[CH:19][CH:11]12.[OH2:21]>>[C:10]([OH:15])(=[O:20])[CH:11]1[CH:19]=[CH:18][CH2:17][CH2:16][CH:12]1[C:13]([OH:21])=[O:14]Participants
Procedure
In a beaker having an inner volume of 2 liters, 800 ml of deionized water was charged and, with stirring pieces immersed therein, was stirred and boiled on a stirrer provided with a hot plate. In this hot water, 12.6 g of melamine was thoroughly dissolved. Separately, in a beaker having an inner volume of one liter, 500 ml of deionized water was charged and, with stirring pieces immersed therein, was stirred and boiled on a stirrer provided with a hot plate. In this hot water, 15.2 g of tetrahydrophthalic anhydride was added and the resultant mixture was stirred for one hour with heating to give an aqueous solution of tetrahydrophthalic acid. This aqueous solution was added to the aqueous melamine solution mentioned above and the resultant mixture was stirred. The resultant mixed solution, when cooled with ice water, precipitates crystals. The crystals were separated by filtration and then dried in a vacuum drier. By the thermal analysis (DSC), the infrared absorption analysis and the titration with KOH performed in the same manner as in Synthesis Example 1, the crystals were confirmed to have formed a salt of melamine and tetrahydrophthalic acid at a molar ratio of 1:1. This salt will be referred to hereinafter as "melamine-THPA salt".
Workup
- additionwas charged and, with stirring pieces
- customboiled on a stirrer
- customprovided with a hot plate
- additionwas charged and, with stirring pieces
- stirringwas stirred
- customboiled on a stirrer
- customprovided with a hot plate
- temperaturewith heating
Sources & evidence
- ORD record
- ord-d1463565b57249b3aa4b635b48e80764
- Source dataset
- uspto-grants-1997_10
- Patent number
- US05677450
Reaction notes
Loading…