Sodium Hydroxide → HCID 178436706, compound

To a stirred solution of ethyl 3-ethyl-1H-pyrazole-5-carboxylate (41.3 g) in methanol (300 ml) was added dropwise 10M sodium hydroxide solution (63 ml) and the mixture heated at reflux for 4 h. The mixture was allowed to cool overnight and then concentrated. The residue was diluted with water (250 ml) and washed with toluene (3×100 ml). The aqueous phase was acidified to pH=4 by the addition of concentrated hydrochloric acid. The resultant precipitate was collected by filtration, washed with water and dried in a vacuum oven at 45° C. to give the title compound (18.4 g) as a buff solid.

1. temperaturethe mixture heated
2. temperatureat reflux for 4 h
3. temperatureto cool overnight
4. concentrationconcentrated
5. additionThe residue was diluted with water (250 ml)
6. washwashed with toluene (3×100 ml)
7. additionThe aqueous phase was acidified to pH=4 by the addition of concentrated hydrochloric acid
8. filtrationThe resultant precipitate was collected by filtration
9. washwashed with water
10. customdried in a vacuum oven at 45° C.

ORD record

ord-fb1b2cbf7b4b4011b735fec2e296f331

Source dataset

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08658635B2