HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 44180311, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 1,2-Ethanediamine, N1,N1,N2-trimethyl- | HCID 67338 | — |
| Reactant | HCID 57813319 | HCID 57813319 | — |
| Product | HCID 44180311 | HCID 44180311 | — |
Reaction Steps
N-{[3′-(Chloromethyl)-6-fluoro-3-biphenylyl]methyl}-N′-{[1,6-diethyl-4-(tetrahydro-2H-pyran-4-ylamino)-1H-pyrazolo[3,4-b]pyridin-5-yl]methyl}-1,3-benzenedicarboxamide (0.034 g, 0.05 mmol) and N,N,N′-trimethyl-1,2-ethanediamine (0.025 g, 0.25 mmol) were combined in THF (1 mL) and microwaved at 150° C. for 1 h. Purification on a Gilson HPLC using a TFA system was followed by passing the product though a quaternary ammonium hydroxide cartridge to give the free base, the title compound, as a white solid. LC-MS m/z 748.8 (M+H)+, 1.43 min (ret time); mp 126-129° C. Analytical HPLC shows 99.1% purity, (ret time 9.788 min).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08067408B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-874d6ec55be146efbbd74236274b8184 |
| Source note | uspto-grants-2011_11 |