Réaction #1099226

Équation de réaction

2-{[2-((E)-{4-[ethyl(2-hydroxyethyl)amino]phenyl}-diazenyl)-4-(1-piperidinyl)-1,3-thiazol-5-yl]methylene}-1H-indene-1,3(2H)-dione

chlorosulfonic acid

→

2-[{4-[(E)-{5-[(1,3-dioxo-1,3-dihydro-2H-inden-2-ylidene)methyl]-4-(1-piperidinyl)-1,3-thiazol-2-yl}diazenyl]phenyl}(ethyl)amino]ethyl Hydrogen Sulfate

Solvants

THF

Conditions de réaction

Traitement

1. 1
   workup.ADDITIONAfter the addition
2. 2
   Températurethe reaction mixture was heated
3. 3
   Températureunder reflux for 4 hours
4. 4
   Températureto cool to room temperature
5. 5
   workup.STIRRINGstirred overnight
6. 6
   TempératureAfter further cooling in an ice bath the formed precipitate
7. 7
   Filtrationwas filtered off
8. 8
   Lavagewashed with a little cold THF
9. 9
   Autredried at 40° C. in vacuum

Mode opératoire

0.32 g (0.62 mmol) 2-{[2-((E)-{4-[ethyl(2-hydroxyethyl)amino]phenyl}-diazenyl)-4-(1-piperidinyl)-1,3-thiazol-5-yl]methylene}-1H-indene-1,3(2H)-dione were dissolved in 33 ml THF and cooled to 0° C. Then 0.11 g (0.93 mmol) chlorosulfonic acid were added slowly drop by drop with stirring. After the addition was completed, the reaction mixture was heated under reflux for 4 hours, allowed to cool to room temperature and stirred overnight. After further cooling in an ice bath the formed precipitate was filtered off, washed with a little cold THF and dried at 40° C. in vacuum.

Source