HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68992044, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 1,1-Dimethylethyl (2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)(1-{2-[7-(methyloxy)-2-oxo-1(2H)-quinolinyl]ethyl}-4-piperidinyl)carbamate | HCID 86635310 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68992044 | HCID 68992044 | 89% |
Reaction Steps
To a solution of 1,1-dimethylethyl (2,3-dihydro[1,4]dioxino[2,3-c]pyridin-7-ylmethyl)(1-{2-[7-(methyloxy)-2-oxo-1(2H)-quinolinyl]ethyl}-4-piperidinyl)carbamate (92 mg) in chloroform (1.5 ml) was added 4N HCl in 1,4-dioxane (1.5 ml) and the reaction stirred at rt for 1 h. More 4N HCl in 1,4-dioxane (0.5 ml) was added and the reaction stirred at rt for 0.5 h then the solvents removed. The residue was dissolved in MeOH (25 ml) and treated with Amberlyst A21 basic resin until the pH was 6. The residue was filtered off and the solvent removed; the residue was subjected to column chromatography on silica gel eluting with 0-20% methanol-DCM to afford the free base of the title compound (67 mg, 89%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071592B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-075e627c0c5d49deafd62383bb96e99f |
| Source note | uspto-grants-2011_12 |