HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-[4-(Bromomethyl)phenyl]ethan-1-one → 6-(4-acetylbenzylthio)-3-tert-butoxycarbonyl-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-[4-(Bromomethyl)phenyl]ethan-1-one | HCID 583785 | — |
| Reactant | 3-tert-butoxycarbonyl-7-chloro-6-dimethylaminocarbonylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine | HCID 57655979 | — |
| Product | 6-(4-acetylbenzylthio)-3-tert-butoxycarbonyl-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine | HCID 57656189 | 82% |
Reaction Steps
Use a method similar to the General Procedure 7 to react 3-tert-butoxycarbonyl-7-chloro-6-dimethylcarbamoylthio-2,3,4,5-tetrahydro-1H-benzo[d]azepine (200 mg, 0.521 mmol) with 4-acetylbenzyl bromide (555 mg, 2.605 mmol). Purify the crude mixture by chromatography on silica gel eluting sequentially with hexane and hexane/EtOAc (9:1, 4:1) to obtain 6-(4-acetyl-benzylthio)-3-tert-butoxycarbonyl-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (190 mg, 82%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08580780B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-d3dccb6190da489e851434cdf65d4489 |
| Source note | uspto-grants-2013_11 |