Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 18444278 | HCID 18444278 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18444277 | HCID 18444277 | 39.9% |
Reaction Steps
To a THF (5 ml) solution of 171 mg of 4-{4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazin-1-yl}benzoic acid was added 63 mg of CDI, followed by stirring at 60° C. Further, 52 mg of CDI was added in twice thereto, and the whole was stirred at 60° C. for 24 hours in total. After the reaction solution was cooled to room temperature, 0.25 ml of aqueous ammonia was added thereto, followed by 6 hours of stirring at room temperature. Further, 0.5 ml of aqueous ammonia was added thereto and the whole was stirred at room temperature. Thus precipitated crude crystals were collected by filtration and recrystallized from methanol-THF to obtain 68 mg of 4-{4-[6-(3,4-dimethoxyphenyl)pyridine-2-carbonyl]piperazin-1-yl}benzamide as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07196080B2 |
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| Source dataset | uspto-grants-2007_03 |
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| ORD ID | ord-eb522da1f1d3484fae47bafe1ca45ae4 |
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| Source note | uspto-grants-2007_03 |
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