Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 67337338 | HCID 67337338 | — |
| Solvent | Ethylacetate methanol | HCID 21584119 | — |
| Product | HCID 16062559 | HCID 16062559 | 94.6% |
Reaction Steps
Add hydrogen chloride into a mixture of 3-tert-butoxycarbonyl-7-chloro-6-[(4-cycloheptylcarbamoyl-phenylamino)-methyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (590 mg, 1.12 mmol) in EtOAc/methanol (1:1, 60 mL) until the mixture is saturated. Stir for 1 h at 40° C. and concentrate in vacuo. Purify the residue by SCX chromatography to obtain 7-chloro-6-[(4-cycloheptylcarbamoyl-phenylamino)-methyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (450 mg, 1.06 mmol). Use a method similar to the General Procedure 2-1 to obtain the title compound as an off-white solid (560 mg, 92%). MS (ES+) m/z: 426 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07994163B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-ce0cf14073cd48558d774647725f2ecf |
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| Source note | uspto-grants-2011_08 |
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