HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → Ivabradine Impurity 1 Hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | 3-(3-Chloropropyl)-7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-one | HCID 13092510 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | Ivabradine Impurity 1 Hydrochloride | HCID 13319974 | — |
Reaction Steps
First, 1-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-3-chloro-propane (5.9 g, 0.020 mol) and methylamine (14 g, 0.45 mol) are heated to 130° C. for 1 hour in a sealed tube. Then, the cooled reaction product is taken up in semi-concentrated sodium hydroxide solution and extracted with methylene chloride. After the extract has been dried and concentrated, the hydrochloride is precipitated from acetone/ether with ethereal hydrochloric acid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04737495 |
| Source dataset | uspto-grants-1988_04 |
| ORD ID | ord-d420edbe2c5f4f03bfb4175b4f2c0689 |
| Source note | uspto-grants-1988_04 |