5-Aminoisophthalic acid synthesis
- Product Name:5-Aminoisophthalic acid
- CAS Number:99-31-0
- Molecular formula:C8H7NO4
- Molecular Weight:181.15
618-88-2
99-31-0
In a 3L four-neck flask equipped with a mechanical stirrer, 211.1 g (1.0 mol, 1.0 eq.) of 5-nitroisophthalic acid and 160.0 g (4.0 mol, 4.0 eq.) of sodium hydroxide were dissolved in 2L of water. A thermometer was installed and the mixture was stirred for 1 hour until the system was clarified. Subsequently, 10 g of Nguyenay nickel was added and the temperature was slowly raised to 30-35°C. At this temperature, 125.0 g (2.0 mol, 2.0 eq.) of 80% hydrazine hydrate was added dropwise for a controlled drop time of 30 minutes. After dropwise addition, stirring was continued for 30 min to ensure complete reaction. At the end of the reaction, the pH of the filtrate was adjusted to 3.5-4.0 with acetic acid and a large amount of white solid was precipitated. The precipitate was collected by filtration and dried to give 172.0 g of 5-aminoisophthalic acid in 95% yield and 99.7% purity.
618-88-2
516 suppliers
$13.00/25g
99-31-0
450 suppliers
$6.00/10g
Yield:99-31-0 95%
Reaction Conditions:
Stage #1:5-nitrobenzene-1,3-dicarboxylic acid with sodium hydroxide in water for 1 h;
Stage #2: with hydrazine hydrate in water at 30 - 35; for 1 h;Concentration;Temperature;
Steps:
2 Example 2:
In a 3 L four-necked flask equipped with a mechanical stirrer, a thermometer was charged 211.1 g (1.0 mol, 1.0 eq) of 5-nitroIsophthalic acid, 160.0 g (4.0 mol, 4.0 eq) of sodium hydroxide in 2 L of water, and the mixture was stirred for 1 hour to clarify the system. Then add 10g of Raney nickel, slowly raise the temperature between 30 ~ 35 , and then drop into the 80% hydrazine hydrate 125.0g (2.0mol, 2.0eq), 30 minutes drop finished, continue stirring for 30 minutes to end the reaction. The pH of the filtrate was adjusted to 3.5 to 4.0 with acetic acid, and a large amount of white solid was precipitated by filtration and dried to obtain 172.0 g of 5-aminoisophthalic acid in a yield of 95% and purity of 99.7% ).
References:
Tianjinxi Zerun Technology Co., Ltd.;Ma, Junli CN106748840, 2017, A Location in patent:Paragraph 0020; 0021; 0022; 0023; 0024; 0025
618-88-2
516 suppliers
$13.00/25g
7440-44-0
348 suppliers
$12.00/25g
99-31-0
450 suppliers
$6.00/10g