Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178510883 | HCID 178510883 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10339105 | HCID 10339105 | — |
Reaction Steps
352 mg (0.91 mmol) of 2-[8-chloro-1-(2-chloro-phenyl)-1H-imidazo[4,5-c]quinolin-2-yl]-N-hydroxy-acetamidine (Example 87), 0.91 ml 1N HCl, in 7.1 ml water are hydrogenated at rt (tlc-control) in the presence of ca. 190 mg Raney-Ni. The catalyst is filtered off and washed with methanol. The solvents are evaporated, the residue is dissolved in CH2Cl2-water-methanol. The two phases are separated and evaporated. From the water phase, a yellow oil separates. The oil is dissolved in hot methanol and diethyl ether is added. On stirring at 0-5° C., a solid separates. The solid, which is the title compound, is filtered off and dried for 6 h at 50° C. MS: 370 (M++1); HPLC: tret=7.38 min (Grad 1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07998972B2 |
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| Source dataset | uspto-grants-2011_08 |
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| ORD ID | ord-e5f96c13c2dd4cbba14d350b05a90ba3 |
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| Source note | uspto-grants-2011_08 |
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