HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 136030690, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 136068494 | HCID 136068494 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 136030690 | HCID 136030690 | 40% |
Reaction Steps
Crude (R)-3-[2-(2-hydroxy-phenyl)-quinazolin-4-yl-amino]-piperidine-1-carboxylic acid tert-butyl ester (˜1.0 mmol) was dissolved in methanol (4 mL) and 4M HCl in dioxane (10 mL) was added. After stirring for 24 hours the solution was concentrated and purified by ion exchange chromatography on SCX-2 Isolute acidic resin (5 g), eluting with methanol and then 1 M ammonia in methanol. Further purification by silica column chromatography, eluting with 20% methanol in dichloromethane, gave the title compound as a yellow solid (0.127 g, 40%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08324226B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-846541e3debf444b87dc0546448568d8 |
| Source note | uspto-grants-2012_12 |