反应详情

A 48.3 g portion of 4-amino-1,5-naphthalenedisulfonic acid sodium salt is suspended in 150 ml of water and 160 ml of 1N sodium hydroxide is added, then 60.0 g of m-nitrobenzoyl chloride is added all at once. The mixture is shaken for about 15 minutes or until no longer basic to test paper, then another 160 ml of 1N sodium hydroxide is added with additional shaking. The latter addition of sodium hydroxide and shaking is repeated two more times and when the mixture remains basic after 1/2 hour of shaking after the last portion is added the mixture is acidified to Congo Red with 15 ml of concentrated hydrochloric acid. Additional water is added to the mixture which is then copiously extracted with ether. The ether is removed by vacuum siphoning and the aqueous phase is filtered. The filtrate is neutralized and is concentrated at 55° C. in vacuo until crystal formation then it is cooled to room temperature. The crystallized material is collected by filtration and is washed with 250 ml of saturated saline, then with two 150 ml portions of 50% ethyl alcohol followed by two 150 ml portions of absolute ethyl alcohol and two 150 ml portions of ethyl ether. The product of the example is then oven dried at 120° C. overnight.

1. stirringshaking
2. waitremains basic after 1/2 hour
3. stirringof shaking after the last portion
4. additionis added the mixture
5. extractionis then copiously extracted with ether
6. customThe ether is removed by vacuum siphoning
7. filtrationthe aqueous phase is filtered
8. concentrationis concentrated at 55° C. in vacuo until crystal formation
9. filtrationThe crystallized material is collected by filtration
10. washis washed with 250 ml of saturated saline
11. customoven dried at 120° C. overnight