HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrogen chloride-ethyl acetate → 9-(Pyridin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrogen chloride-ethyl acetate | HCID 21866389 | — |
| Reactant | tert-butyl 9-(pyridin-4-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate | HCID 68577733 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 9-(Pyridin-4-yl)-2,3,4,5-tetrahydro-1,4-benzoxazepine dihydrochloride | HCID 68578552 | 19% |
Reaction Steps
A mixture of tert-butyl 9-(pyridin-4-yl)-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate (109 mg, 0.334 mmol), ethyl acetate (1 ml) and 4N hydrogen chloride-ethyl acetate solution (4 ml) was stirred for 1 hr at room temperature, and the solvent was evaporated under reduced pressure. The residue was recrystallized from methanol to give the desired product (19.0 mg, 19.0%) as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247403B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-c238b60f29504fb7905728347146d18c |
| Source note | uspto-grants-2012_08 |