HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 68725893, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68727626 | HCID 68727626 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68725893 | HCID 68725893 | 87.4% |
Reaction Steps
To a suspension of methyl-5-{[({1-[4-(trifluoromethyl)pyrimidin-2-yl]piperidin-4-yl}methyl)amino]carbonyl}pyridine-2-carboxylate (272 mg, 0.643 mmol) in tetrahydrofuran, methanol, and water (5 ml, in a ratio of 3:2:1, respectively) was added lithium hydroxide (108 mg, 2.57 mmol). The reaction was stirred at ambient temperature for 18 h and then concentrated in vacuo to afford the title compound as a white solid (230 mg). Mass spectrum (ESI) 410 (M+1). 1H NMR (500 MHz, CD3OD) δ 8.96 (s, 1H), 8.54 (d, 1H, J=4.8 Hz), 8.24 (d, 1H, J=8.3 Hz), 8.05 (d, 1H, J=8 Hz), 6.81 (d, 1H, J=4.8 Hz), 4.70-5.0 (m, 2H), 2.94-3.01 (m, 2H), 1.97-2.03 (m, 1H), 1.88 (d, 2H, J=12.8 Hz), 1.21-1.34 (m, 4H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08445480B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-a93b604e3878489cbc6942cf6517a12d |
| Source note | uspto-grants-2013_05 |