HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | N-Demethylivabradine | HCID 10389261 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 3-(3-(((7S)-3,4-dimethoxy-7-bicyclo(4.2.0)octa-1,3,5-trienyl)methylamino)propyl)-7,8-dimethoxy-2,5-dihydro-1H-3-benzazepin-4-one;hydrochloride | HCID 66672699 | 72.1% |
Reaction Steps
300 mg (0.65 mmol) of the amine obtained in Example 2, Step 2, are dissolved in 10 mL of acetonitrile. To the resulting solution there is added 0.65 mL (1.3 mmol, 2 equivalents) of 2M hydrochloric acid solution in diethyl ether. Stirring is carried out at 25° C. for 15 minutes, and then evaporation to dryness. The product is crystallised from 20 mL of acetone. The solid is filtered off and dried. 230 mg of white crystals are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101747B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-2d9610d533be42abacb334f404b541fb |
| Source note | uspto-grants-2012_01 |