Hydrochloric Acid → HCID 23329521, compound
Reaction equation
Br[CH2:2][CH2:3][N:4]1[CH:8]=[C:7]([C:9]([NH2:11])=[O:10])[C:6]([N+:12]([O-:14])=[O:13])=[N:5]1.C([O-])([O-])=O.[Na+].[Na+].Cl>>[N+:12]([C:6]1[C:7]([C:9]([NH2:11])=[O:10])=[CH:8][N:4]([CH:3]=[CH2:2])[N:5]=1)([O-:14])=[O:13]Participants
4
Procedure
A suspension of 5 gm. of 1-(2-bromoethyl)-3-nitro-4-pyrazolecarboxamide in 100 ml. of 5 percent Na2CO3 solution was refluxed with stirring for 5 hours. The mixture was cooled in an ice bath and acidified to ph 2 with concentrated HCl. The product precipitated and was separated by filtration. The solids were washed with cold water and recrystallized from methanol-water to product 2 gm. of 3-nitro-1-vinyl-4-pyrazolecarboxamide, m.p. 150°-52° C.
Workup
- additionA suspension of 5 gm
- temperatureThe mixture was cooled in an ice bath
- customThe product precipitated
- customwas separated by filtration
- washThe solids were washed with cold water
- customrecrystallized from methanol-water to product 2 gm
Sources & evidence
- ORD record
- ord-e315e7fb04fe4863a6d28450b0de887b
- Source dataset
- uspto-grants-1980_11
- Patent number
- US04235995
Reaction notes
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