HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane hydrochloride → HCID 117697385, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 117700211 | HCID 117700211 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 117697385 | HCID 117697385 | 110.6% |
Reaction Steps
To a solution of (1R,5R,6R)-tert-butyl 6-(2-ethoxy-2-oxoethoxy)-3-oxa-8-azabicyclo[3.2.1]octane-8-carboxylate 50a (racemic, 200 mg, 0.63 mmol) in DCM (10 mL) was added HCl/dioxane (2 mL, 7 M). The resulting mixture was stirred at room temperature for 2 h. The organic solvent was removed in vacuo to give the compound 50b (150 mg, 94%). MS: calc'd (MH+) 216, measured (MH+) 216; 1H NMR (CDCl3, 400 MHz): 4.28 (m, 8H), 3.79 (m, 1H), 3.70 (s, 1H), 3.57 (d, J=12.4 Hz, 1H), 2.50 (m, 1H), 2.31 (m, 1H), 1.28 (m, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09266904B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-f80a7add113f455c808fb7b791831e87 |
| Source note | uspto-grants-2016_02 |