HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22903535, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium hydrido[tris(methanolato)]borate(1-) | HCID 3084262 | — |
| Reactant | HCID 22903504 | HCID 22903504 | — |
| Solvent | 1,2-Dimethoxyethane | HCID 8071 | — |
| Product | HCID 22903535 | HCID 22903535 | 48.6% |
Reaction Steps
To a solution of 7-chloro-1-{6-[2-(3-ethoxycarbonylpropoxy)benzoylamino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (2.5 g) in ethylene glycol dimethyl ether (70 ml) is added sodium trimethoxyborohydride (3.78 g), and the mixture is refluxed for 3 hours. The reaction solution is gradually poured into diluted hydrochloric acid, and the mixture is extracted with ethyl acetate. The extract is washed with water, dried over magnesium sulfate, and evaporated under reduced pressure to remove the solvent. The residue is purified by silica gel column chromatography, and recrystallized from dichloromethane-diethyl ether to give 7-chloro-1-{6-[2-(4-hydroxybutoxy)benzoylamino]nicotinoyl}-2,3,4,5-tetrahydro-1H-benzazepine (1.12 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05677299 |
| Source dataset | uspto-grants-1997_10 |
| ORD ID | ord-bc9b3b8aed2e417c8fd4dbd4636f0add |
| Source note | uspto-grants-1997_10 |