Reacción #93123

Ecuación de reacción

sodium azide

sodium 4-sulfophenylisothiocyanate

( 1 )

sodium 4-sulfophenylisothiocyanate

→

Compound

Rendimiento 25.0%

1-(4-Sulfophenyl)-5-mercaptotetrazole sodium salt

Rendimiento 25.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONabove was added
2. 2
   TemperaturaThe resulting mixture was heated
3. 3
   Otrofor 8 hours
4. 4
   Otroby removing solids
5. 5
   Filtraciónby filtration
6. 6
   workup.ADDITIONAfter adding 125 ml of 20% sulfuric acid to the filtrate, it
7. 7
   Concentraciónwas concentrated under reduced pressure
8. 8
   workup.ADDITIONAddition of 20 g of NaCl to the concentrate
9. 9
   Otroprecipitation of crystals
10. 10
    FiltraciónThe crystals were collected by filtration
11. 11
    workup.DISSOLUTIONdissolved in a mixed solution of 80 ml of water and 20 ml of 2N HCl
12. 12
    workup.ADDITIONAddition of NaCl
13. 13
    Otroprecipitation of crystals
14. 14
    FiltraciónThe crystals were collected by filtration
15. 15
    Otrodried

Procedimiento

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.

Fuente