Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Formaldehyde | HCID 712 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | HCID 21488689 | HCID 21488689 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 21488688 | HCID 21488688 | — |
Reaction Steps
An autoclave was charged with 52.1 g (0.1 mole) of 1-phenyl-3-(α-sulphostearoylamino)-2-pyrazolin-5-one, 15.4 g (0.2 mole) of ammonium acetate, 4.5 g (0.15 mole) of paraformaldehyde, 10 g of Raney nickel and 535 ml of ethanol. The mixture was heated to 75° C whereupon hydrogenation started at a hydrogen pressure of 700 psi. After 30 min the hydrogen pressure was released and another 4.5 g of paraformaldehyde were added whereupon hydrogenation was continued. After having filtered off the catalyst, the filtrate was acidified with 100 ml of concentrated hydrochloric acid. The precipitate was filtered off. Yield: 41 g (75%). Melting point: 240° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US04000156 |
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| Source dataset | uspto-grants-1976_12 |
|---|
| ORD ID | ord-194453e4d9754ad2a93f27c86f8092f3 |
|---|
| Source note | uspto-grants-1976_12 |
|---|
