Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | HCID 178527718 | HCID 178527718 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 178508386 | HCID 178508386 | — |
Reaction Steps
65 mg of 7-[2-(6-phenyl-3H-imidazo[4,5-b]pyridin-2-yl)-ethyl]-azepan-2-thione (compound A1) are suspended in 4.3 ml of methanol containing ammonia (strength: 7.0 M) and heated at 50° C. for 90 hours. Subsequently, the reaction mixture is evaporated to dryness and purified by flash chromatography on LiChroprep-NH2® (eluent gradient: dichloromethane/0-100 vol. % methanol), and lyophilized from 2.0 ml of water, 5.0 ml of dioxane to afford 29.5 mg of the title compound as an amorphous, colorless solid of m.p. 117° C. (decomp.). ESI-MS: 334.3 (MH+). TLC: Rf=0.35 (LiChroprep-NH2® HPTLC, methanol/water 10:1 parts by volume).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07790710B2 |
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| Source dataset | uspto-grants-2010_09 |
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| ORD ID | ord-51547afed8134322bacb0dde7e9ab27d |
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| Source note | uspto-grants-2010_09 |
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