HuagongsheHuagongshe Chemistry Print Report · For research reference only
Di-tert-butyl dicarbonate → tert-butyl 7-nitro-2,3,4,5-tetrahydro-1H-3-benzazepine-3-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | 7-Nitro-2,3,4,5-tetrahydro-1H-benzo[D]azepine | HCID 11310042 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | tert-butyl 7-nitro-2,3,4,5-tetrahydro-1H-3-benzazepine-3-carboxylate | HCID 21918821 | 91.7% |
Reaction Steps
To a solution of 7-nitro-2,3,4,5-tetrahydro-1H-3-benzazepine (2.33 g) in dry DCM (120 ml, TEA (4.2 ml 2.5 eq), BOC2O (6.1 g, 2.3 eq.), DMAP (296 mg, 0.2 eq.) were added. The mixture was stirred at rt. for 1 h then the solvent was evaporated in vacuo. The material thus obtained was purified by flash chromatography over silica gel (eluting with 20% ethyl acetate in hexane) to give the title compound (3.25 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989444B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-60a14de9775f475e9bb7329c08d493f9 |
| Source note | uspto-grants-2011_08 |