HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 68993634, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 86635316 | HCID 86635316 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68993634 | HCID 68993634 | 55.1% |
Reaction Steps
1,1-dimethylethyl {1-[2-(9-oxo-2,3-dihydro[1,4]dioxino[2,3-h]quinolin-10(9H)-yl)ethyl]-4-piperidinyl}carbamate (1 g; 2.34 mmol) was dissolved in chloroform (8 ml) and 4M HCl in 1,4-dioxane (10 ml) added. This was then stirred at rt for 1 h. The salts from the reaction were dissolved in MeOH and all solvents then removed. The residues were redissolved in MeOH and stirred with amberlyst ion exchange resin until a neutral pH was reached. The resin was filtered off and all solvents were removed. The crude residues were subjected to column chromatography on silica gel using a 0-20% 2M NH3: MeOH/DCM gradient to give the desired product (425 mg; 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071592B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-56671d95d422426fa61f776e04f7c6ca |
| Source note | uspto-grants-2011_12 |