Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | HCID 86749345 | HCID 86749345 | — |
| Product | HCID 67769616 | HCID 67769616 | — |
Reaction Steps
To a solution of 7-chloro-5-(4-t-butoxycarbonyl-1-piperazinyl)-carbonylmethyl-1-[6-(2-chlorobenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine (1.2 g)in dioxane (20 ml)is added 5 N hydrochloric acid (2 ml), and the mixture is stirred at room temperature overnight. Water is added to the reaction mixture, and the mixture is made basic with aqueous sodium hydroxide solution, and extracted with dichloromethane. 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 ethyl acetate-diethyl ether to give 7-chloro-5-(1-piperazinyl)carboxymethyl-1-[6-(2-chlorobenzoylamino)nicotinoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.54 g) as white powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05498609 |
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| Source dataset | uspto-grants-1996_03 |
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| ORD ID | ord-f746ea66658e41e8a3cd4d39c19e3730 |
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| Source note | uspto-grants-1996_03 |
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