反应详情

温度

95 °C

To a stirred solution of 4.0 g of 8,8'-[(5-amino-1,3-phenylene)bis(carbonylimino)]di-1,3,6-naphthalenetrisulfonic acid, hexasodium salt in 50 ml of water is added 4.0 ml of 3-trifluoromethylphenyl isocyanate. Stirring is continued for 6 hours at room temperature then the resulting mixture is heated to 95° C, is filtered through diatomaceous earth and washed with 50 ml of hot water. The hot filtrate is salted with 55 g of sodium acetate trihydrate and after standing for 40 hours is diluted with 700 ml of anhydrous ethanol. The precipitate is filtered and washed with absolute ethanol and ether. The product is then boiled and triturated with 100 ml of absolute ethanol, cooled to room temperature and is filtered and washed with absolute ethanol followed by ether to give 8,8'-{{5-[3-(α,α,α-trifluoro-m-tolyl)ureido]-1,3-phenylene}bis(carbonylimino)}di-1,3,6-naphthalenetrisulfonic acid, hexasodium salt.

1. filtrationis filtered through diatomaceous earth
2. washwashed with 50 ml of hot water
3. waitafter standing for 40 hours
4. additionis diluted with 700 ml of anhydrous ethanol
5. filtrationThe precipitate is filtered
6. washwashed with absolute ethanol and ether
7. customtriturated with 100 ml of absolute ethanol
8. temperaturecooled to room temperature
9. filtrationis filtered
10. washwashed with absolute ethanol