Sodium Hydroxide → HCID 178514232, compound

Temperature

45 °C

A solution was made of 8 gm. of 1-sodium salt of 3-nitro-4-pyrazolecarbonitrile in methanol, and 75 ml. of 15% H2 O2 was added, followed by 5 ml. of 6N NaOH. The reaction mixture was heated to 45° C., at which point external cooling was needed to maintain the mixture at 45°-50° C. After the exothermic reaction has subsided, the mixture was held at 45°-50° C. and stirred for 4 hours. Then the mixture was cooled and the methanol was evaporated under vacuum. The liquid remaining was cooled in an ice bath and the product was separated by filtration and dried under vacuum. The dry product was determined to be 8 gm. of 3-nitro-4-pyrazolecarboxamide sodium salt, m.p. >300° C.

1. temperatureexternal cooling
2. temperatureto maintain the mixture at 45°-50° C
3. customAfter the exothermic reaction
4. customwas held at 45°-50° C.
5. temperatureThen the mixture was cooled
6. customthe methanol was evaporated under vacuum
7. temperatureThe liquid remaining was cooled in an ice bath
8. customthe product was separated by filtration
9. customdried under vacuum

ORD record

ord-834a5ae2346244a9b51709223828ab1d

Source dataset

uspto-grants-1979_03

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04145554