Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trimethylsilyl isocyanate | HCID 70696 | — |
| Reactant | HCID 68972633 | HCID 68972633 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 58833734 | HCID 58833734 | — |
Reaction Steps
Trimethylsilylisocyanate (0.225 mL, 1.67 mmol) was added dropwise to a slurry of 2-(2-methoxyethyl)-7-(piperidin-4-yloxy)-1-propyl-1H-imidazo[4,5-c]quinolin-4-ylamine (prepared as described in Part A of Example 388, 0.640 g, 1.67 mmol) in chloroform (16 mL) at 0° C. The reaction mixture was stirred for 40 minutes and water (10 mL) was added. The reaction mixture was stirred vigorously for 2 hours, diluted with 200 mL ethanol, and then concentrated under reduced pressure to approximately 100 mL. Another 100 mL ethanol was added and the solution was evaporated to afford a white solid that was recrystallized from ethanol to provide 0.625 g of 4-{[4-amino-2-(2-methoxyethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-7-yl]oxy}piperidine-1-carboxamide as granular off-white crystals, mp 207-208.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08871782B2 |
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| Source dataset | uspto-grants-2014_10 |
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| ORD ID | ord-1c6c552e62064a9bb73b58f9f7357047 |
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| Source note | uspto-grants-2014_10 |
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