Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Sodium Azide | HCID 33557 | — |
| Reactant | HCID 10203446 | HCID 10203446 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178492069 | HCID 178492069 | 9% |
Reaction Steps
To 1-(4-methoxyphenyl)-7-oxo-6-[4-(2-oxo-1(2H)-pyridinyl)phenyl]-4,5,6,7-tetrahydro-1H-pyrazolo[3,4-c]pyridine-3-carbonitrile (0.1 g, 0.23 mmol) in DMF (2 mL) was added NaN3 (19 mg, 0.29 mmol) and NH4Cl (21 mg, 0.38 mmol) and the reaction was heated to 105° C. for 24 h. The reaction was cooled, water (1 mL) was added, and the resulting solid filtered off and dried. The solid was placed in DMF (1 mL) and trityl chloride (60 mg, 0.2 mmol) and pyridine (0.2 mL) were added and stirred for 24 h. The reaction was quenched with water, extracted with EtOAc, and dried (Na2SO4). Purification on silica gel was not successful. The trityl group was removed with TFA (0.5 mL) in CH2Cl2 for 2 h. The solvents were removed and the compound was purified by HPLC and freeze-dried to afford 10 mg (9%) of a white solid; High Resolution Mass Spec (M+H)+ for C25H21N8O3 481.1749.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07960411B2 |
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| Source dataset | uspto-grants-2011_06 |
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| ORD ID | ord-76252d04f5c54f08a777b8e5233d92a1 |
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| Source note | uspto-grants-2011_06 |
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