HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitric Acid → HCID 59150535, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Ammonium Hydroxide | HCID 14923 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 57505967 | HCID 57505967 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59150535 | HCID 59150535 | 67% |
Reaction Steps
Nitric acid (65%, 0.370 ml) was added dropwise with vigorous stirring to 1,1-dimethylethyl 7-hydroxy-6-methyl-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carboxylate (600 mg) and silica gel (1.67 g) in DCM (5.7 ml) at −15° C. After 30 min a mixture of DCM/MeOH/conc.NH4OH: 10/3/1.5 was added and silica gel was filtered off. The solvent was evaporated under reduced pressure and the residue was purified on silica gel (ethyl acetate/petroleum ether: 15/85) obtaining the desired compound (470 mg, 67% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989444B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-66326866d8e94465b96685838e4162ad |
| Source note | uspto-grants-2011_08 |