HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonia → HCID 19707339, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Phenylacetic Acid | HCID 999 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 19707357 | HCID 19707357 | — |
| Solvent | Ethylene Glycol | HCID 174 | — |
| Solvent | Diglyme | HCID 8150 | — |
| Product | HCID 19707339 | HCID 19707339 | — |
| Product | HCID 53780108 | HCID 53780108 | — |
Reaction Steps
By following the procedures described in Example 40, Steps A, B, C, D, E and F using phenylacetic acid as the starting material and in Step F using methylamine rather than ammonia and diglyme rather than ethylene glycol, the compound 4-methyl-10b-methyl-1,2,3,4,6,10b-hexahydrobenzo[f]quinolin-3-one was prepared. This hexahydrobenzo[f]quinolin-3-one was hydrogenated by following the procedures described in Example 22 except that the reaction was carried out at 60° C. over 7 hours. The reaction mixture was filtered and solvent evaporated under vacuum. The residue was purified by chromatography on SiO2 (CHCl3 as eluent) followed by recrystallization from ethyl acetate/hexanes to afford 154 mg of the title compound. Melting point 111°-113° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05239075 |
| Source dataset | uspto-grants-1993_08 |
| ORD ID | ord-ec65e3214a5b4d2180d01108b504369e |
| Source note | uspto-grants-1993_08 |