Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68998082 | HCID 68998082 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 68999956 | HCID 68999956 | 51% |
Reaction Steps
To a solution of (S)—N-(1-azabicyclo[2.2.2]oct-3-yl)-2-(2-methylcyclopropyl)benzoxazole-4-carboxamide (149 mg, 0.45 mmol) in methanol (0.5 mL) was added a solution of HCl in diethyl ether (1 N, 0.92 mL, 0.92 mmol) at room temperature slowly. The reaction mixture was diluted with diethyl ether. The resulting solid was filtered and washed with diethyl ether to afford (S)—N-(1-azabicyclo[2.2.2]oct-3-yl)-2-(2-methylcyclopropyl)benzoxazole-4-carboxamide hydrochloride (82 mg, 51%) as a white solid and as a mixture of diastereomers: 1H NMR (500 MHz, DMSO-d6) δ 12.68 (br s, 1H), 9.51 (br s, 1H), 8.12 (d, J=8.0 Hz, 1H), 7.68 (d, J=8.0 Hz, 1H), 7.38 (t, J=7.9 Hz, 1H), 4.69-4.58 (m, 1H), 3.80-3.70 (m, 1H), 3.50-3.20 (m, 5H), 2.60-2.50 (m, 1H), 2.40-2.35 (m, 1H), 2.25-1.95 (m, 4H), 1.65-1.60 (m, 1H), 1.50-1.42 (m, 1H), 1.35-1.30 (m, 2H), 1.17-1.10 (m, 2H); MS (ESI+) m/z 326 (M+H); HPLC 98.9% (AUC), tR=11.59 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08278301B2 |
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| Source dataset | uspto-grants-2012_10 |
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| ORD ID | ord-c3cf78811e484720a98a332600938fe2 |
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| Source note | uspto-grants-2012_10 |
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