反应详情

To a stirred solution of 3.62 g of 5-aminoisophthalic acid and 1.85 g of sodium bicarbonate in 80 ml of water plus 7.8 ml of 5N sodium hydroxide is added 11.24 g of crude 5,5'-[6-chloro-s-triazine-2,4-diyl)diimino]diisophthalic acid tetrasodium salt (prepared as described in Example 2). The reaction mixture is refluxed for 15 hours, then is filtered. The filtrate is diluted with 100 ml of absolute ethanol to give a precipitate. The precipitate is collected by filtration and is washed with (8:10) aqueous ethanol, 75% aqueous ethanol, ethanol and ether to give 14.2 g of crude product. The product is warmed with 80 ml of water and 0.1 ml of 5N sodium hydroxide is added to achieve pH 9. The mixture is filtered through diatomaceous earth and the filtrate is diluted with 100 ml of absolute ethanol with formation of a thick paste on stirring. The paste is filtered, stirred in absolute ethanol and filtered again, then is washed with ether and dried by conventional means to give a 9.9 g of a colorless powder as the product of the example.

1. temperatureThe reaction mixture is refluxed for 15 hours
2. filtrationis filtered
3. additionThe filtrate is diluted with 100 ml of absolute ethanol
4. customto give a precipitate
5. filtrationThe precipitate is collected by filtration
6. washis washed with (8:10) aqueous ethanol, 75% aqueous ethanol, ethanol and ether
7. customto give 14.2 g of crude product
8. additionis added
9. filtrationThe mixture is filtered through diatomaceous earth
10. additionthe filtrate is diluted with 100 ml of absolute ethanol with formation of a thick paste
11. filtrationThe paste is filtered
12. stirringstirred in absolute ethanol
13. filtrationfiltered again
14. washis washed with ether
15. customdried by conventional means