Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 86733646 | HCID 86733646 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86733645 | HCID 86733645 | — |
Reaction Steps
2,7 g of iron turnings are added to a hot solution of 2.0 g of cis-1,2,3,4,4a,10b-hexahydro-8,9-dimethoxy-2-methyl-6-(4-nitrophenyl)-benzo[c][1,6]naphthyridine in 40 cc of ethanol and 13 cc of water. A mixture of 13 cc of ethanol, 3 cc of water and 0.7 cc of 2 N hydrochloric acid is added dropwise within 40 minutes while heating, and the reaction mixture is boiled under reflux for a further 3 hours. 1 cc of a 2 N caustic soda solution is then added, filtration is effected and the filtrate is concentrated by evaporation in a vacuum. The residue is dissolved in chloroform, the solution is dried over sodium sulphate, filtered and concentrated by evaporation in a vacuum. The residue is crystallized from ethyl acetate, whereby yellowish prisms having a M.P. of 168°-170°, are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US03966938 |
|---|
| Source dataset | uspto-grants-1976_06 |
|---|
| ORD ID | ord-9c38e1a9588443ceae76cf0da46d6ad5 |
|---|
| Source note | uspto-grants-1976_06 |
|---|