Reaktion #1093842

Reaktionsgleichung

product

(R)-2-(2,4-Difluorophenyl)-3-(4-iodophenyl)-1-(1H-1,2,4-triazol-1-yl)-3-buten-2-ol (+)-3-bromocamphor-10-sulphonate

NaOH

→

solid

Ausbeute 96.3%

(R)-2-(2,4-Difluorophenyl)-3-(4-iodophenyl)-1-(1H-1,2,4-triazol-1-yl)-3-buten-2-ol

Ausbeute 96.3%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeseparated
2. 2
   ExtraktionThe aqueous phase was re-extracted with methylene chloride (310 ml)
3. 3
   WaschenThe organic product solution was washed with water (620 ml)
4. 4
   Einengenconcentrated to a volume of 245 ml
5. 5
   workup.STIRRINGTo the stirred
6. 6
   Einengenseeded concentrate at room temperature
7. 7
   workup.ADDITIONwas added hexane (2450 ml) at a steady rate
8. 8
   workup.WAITThe resulting slurry was granulated at 5° C. for 1 hour
9. 9
   FiltrationFiltration

Vorschrift

The product of step (g) (206.5 g, 0.27 moles) was added to methylene chloride (620 ml) and basified with 40% NaOH. The mixture was stirred for 15 minutes at room temperature and separated. The aqueous phase was re-extracted with methylene chloride (310 ml). The organic product solution was washed with water (620 ml) and concentrated to a volume of 245 ml. To the stirred and seeded concentrate at room temperature was added hexane (2450 ml) at a steady rate. The resulting slurry was granulated at 5° C. for 1 hour. Filtration afforded a white solid (117.4 g, 0.26 moles) which was characterized by 1H NMR spectroscopy.

Quelle