反应详情

To a stirred solution of 10.0 g of 2-(m-aminobenzamido)-1,5-naphthalenedisulfonic acid disodium salt prepared as in Example 2) and 22.4 g of anhydrous sodium carbonate in 250 ml of water is bubbled in phosgene at room temperature for 35 minutes before a thick translucent gel is formed. The gas diffuser is removed and stirring speed is increased considerably. The resulting mixture is changed to a white solid after about 20 minutes of stirring (at this point the mixture is not acid to Congo Red). The gas diffuser is reinserted and phosgenation is continued for an additional hour at room temperature then the acid mixture is neutralized with 12 ml of 3N sodium hydroxide. The mixture is then filtered over a 48 hour period to obtain a moist paste which is slurried with about 125-150 ml of 80% ethyl alcohol then is filtered and is oven dried at 120° C. overnight to give the product of the example.

1. customis bubbled in phosgene at room temperature for 35 minutes before a thick translucent gel
2. customis formed
3. customThe gas diffuser is removed
4. temperatureis increased considerably
5. stirringof stirring (at this point the mixture
6. waitphosgenation is continued for an additional hour at room temperature
7. filtrationThe mixture is then filtered over a 48 hour period
8. customto obtain a moist paste which
9. filtrationthen is filtered
10. customdried at 120° C. overnight
11. customto give the product of the example