反应详情

19.5 g of sodium azide was dissolved in 1.5 l of water, then 23.7 g of sodium 4-sulfophenylisothiocyanate synthesized in (1) above was added thereto. The resulting mixture was heated using a steam bath for 8 hours, followed by removing solids by filtration. After adding 125 ml of 20% sulfuric acid to the filtrate, it was concentrated under reduced pressure. Addition of 20 g of NaCl to the concentrate caused precipitation of crystals. The crystals were collected by filtration, then dissolved in a mixed solution of 80 ml of water and 20 ml of 2N HCl. Addition of NaCl thereto little by little caused precipitation of crystals. The crystals were collected by filtration and dried to obtain 7 g of Compound II-1.

1. additionabove was added
2. temperatureThe resulting mixture was heated
3. customfor 8 hours
4. customby removing solids
5. filtrationby filtration
6. additionAfter adding 125 ml of 20% sulfuric acid to the filtrate, it
7. concentrationwas concentrated under reduced pressure
8. additionAddition of 20 g of NaCl to the concentrate
9. customprecipitation of crystals
10. filtrationThe crystals were collected by filtration
11. dissolutiondissolved in a mixed solution of 80 ml of water and 20 ml of 2N HCl
12. additionAddition of NaCl
13. customprecipitation of crystals
14. filtrationThe crystals were collected by filtration
15. customdried