Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Piperidine | HCID 8082 | — |
| Reactant | Cyclopropanecarboxaldehyde | HCID 123114 | — |
| Reactant | HCID 71015768 | HCID 71015768 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86714502 | HCID 86714502 | 32% |
Reaction Steps
Into a 50 mL round-bottom flask, was placed a solution of 3-[(2R)-2-([4-amino-3-[4-(2-fluorophenoxy)phenyl]-1H-pyrazolo[3,4-d]pyrimidin-1-yl]methyl)pyrrolidin-1-yl]-3-oxopropanenitrile (50 mg, 0.11 mmol, 1.00 equiv) in methanol (10 mL), piperidine (50 mg, 0.59 mmol, 6.73 equiv), and cyclopropanecarbaldehyde (50 mg, 0.71 mmol, 5.54 equiv). The resulting solution was stirred for 1 h at room temperature and then concentrated under vacuum. The residue was loaded onto a silica gel column and eluted with dichloromethane/methanol (100:1, 50:1) to give 0.0179 g (32%) of the title compounds as an off-white solid. LC-MS (ES, m/z): 524 [M+H]+, 1HNMR (300 MHz, CDCl3, ppm) 8.396 (1H, s), 7.689˜7.628 (2H, m), 7.284˜7.085 (6H, m), 6.825˜6.798 (1H, d); 5.663 (2H, s); 4.868 (1H, d); 4.676 (2H, d); 3.708˜3.470 (2H, m); 2.060˜1.980 (5H, m); 1.226 (2H, t); 0.873 (2H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08759358B1 |
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| Source dataset | uspto-grants-2014_06 |
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| ORD ID | ord-bcdff259eb254dc4bdd8a640d673b4b8 |
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| Source note | uspto-grants-2014_06 |
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