HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 59787387, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | HCID 59787401 | HCID 59787401 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59787387 | HCID 59787387 | 55.5% |
Reaction Steps
Dissolve 3-tert-butoxycarbonyl-7-chloro-6-[5-(cyclopentanecarbonyl-amino)-pentyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (311 mg, 0.67 mmoles) in dichloromethane (10 mL) and add trifluoroacetic acid (3 mL). Stir the reaction for 1 h. Concentrate in vacuo and purify the residue by preparative HPLC to give 7-chloro-6-[5-(cyclopentanecarbonyl-amino)-pentyl]-2,3,4,5-tetrahydro-1H-benzo[d]azepine (135 mg) as an oil. Dissolve the oil in methanol (5 mL) and add (L)-tartaric acid (56 mg, 0.37 mmoles). Concentrate the mixture in vacuo and then add water (5 mL). The resulting solution is then freeze dried overnight to yield the title compound as a white solid (184 mg, 55%). MS (ES+) m/z=363.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08420631B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-5c1a20cef71542b2809228ba71de17da |
| Source note | uspto-grants-2013_04 |