HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Bromide → HCID 59787403, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Bromide | HCID 82050 | — |
| Reactant | 3-tert-Butoxycarbonyl-7-chloro-6-chloromethyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine | HCID 59787410 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59787403 | HCID 59787403 | 85.2% |
Reaction Steps
Combine 3-tert-butoxycarbonyl-7-chloro-6-chloromethyl-2,3,4,5-tetrahydro-1H-benzo[d]azepine (3.17 g, 8.14 mmol) and lithium bromide (0.98 g, 11.3 mmol) in anhydrous THF (60 mL) and stir at room temperature for 1 h. Concentrate in vacuo and partition the residue between dichloromethane/water. Dry the organic phase over Na2SO4, filter and concentrate in vacuo. Purify the crude mixture by chromatography on silica gel eluting with hexane/EtOAc (1:0 and 10:1) to obtain the title compound as a white solid (2.6 g, 85%). MS (APCI+) m/z: 274 (M-Boc+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994163B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-2fdd266caad144cc8c0d268d4e105a70 |
| Source note | uspto-grants-2011_08 |