Sodium Hydroxide → 1-Benzyl-1,2,3-triazole

A stirred mixture of 1-benzyl-(1H)-1,2,3-triazole hydrogen chloride (80 g 0.41 moles) in water (320 ml) and ethyl acetate (320 ml) was basified with 20% NaOH (91 ml). The mixture was stirred at room temperature for 10 minutes and separated. The aqueous phase was re-extracted with ethyl acetate (160 ml) and the combined organic product solutions were washed with water (160 ml). The product solution was concentrated to a volume of 195 ml and cooled to room temperature. To the stirred ethyl acetate concentrate was added hexane (585 ml) over 15 minutes. The resulting seeded slurry was granulated at 0° C. for 1 hour. The-filtered white solid (62,4 g, 0.39 moles) was characterised by 1H-NMR spectroscopy.

1. customseparated
2. extractionThe aqueous phase was re-extracted with ethyl acetate (160 ml)
3. washthe combined organic product solutions were washed with water (160 ml)
4. concentrationThe product solution was concentrated to a volume of 195 ml
5. temperaturecooled to room temperature
6. concentrationTo the stirred ethyl acetate concentrate
7. additionwas added hexane (585 ml) over 15 minutes
8. waitwas granulated at 0° C. for 1 hour

ORD record

ord-a898560337044180b74bb627cf3dfe57

Source dataset

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06015825