HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phenylhydrazine hydrochloride → HCID 178478212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phenylhydrazine hydrochloride | HCID 60962 | — |
| Reactant | HCID 178499087 | HCID 178499087 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178478212 | HCID 178478212 | 92% |
Reaction Steps
127 G (1 mole) of caprolactim-methyl-ether were added dropwise over the course of 30 minutes to a mixture of 144.5 g (1 mole) of phenylhydrazine hydrochloride and 700 ml of anhydrous ethanol at -10°C, while stirring well and cooling; the mixture was kept for a further hour at -10°C, then for 2 hours at room temperature and for 30 minutes at the reflux temperature. After cooling, the mixture was filtered and further crystal fractions were isolated by concentrating the mother liquor under reduced pressure. Recrystallization from 5 parts of ethanol yielded 220 g (92% of theory) of caprolactam-phenylhydrazone hydrochloride as almost colorless crystals of melting point 244° to 246°C (with decomposition).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US03936444 |
| Source dataset | uspto-grants-1976_02 |
| ORD ID | ord-2028e9cf9bb540e88ad093af4526bea8 |
| Source note | uspto-grants-1976_02 |