HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium hydroxide, monohydrate → HCID 11681260, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Reactant | HCID 69230482 | HCID 69230482 | — |
| Solvent | Ethanol tetrahydrofuran water | HCID 18504229 | — |
| Product | HCID 11681260 | HCID 11681260 | 41% |
Reaction Steps
Part B. A solution of ethyl 4-[2-(4-isopropyl-phenyl)-pyrimidin-4-yl]-benzoate in THF-water-ethanol (2 mL/2 mL/1 mL) is treated with lithium hydroxide hydrate (60 mg) and stirred for 12 h. The solution is evaporated, and the residue is partitioned between 1 M aq. HCl and ethyl acetate. The organic phase is washed with water (20 mL), dried over magnesium sulfate, filtered and evaporated to afford the title compound as a white solid (65 mg, 41%), m.p. 262-264° C. 1H NMR (300 MHz, acetone-d6): δ 8.96 (1H, d, J=6 Hz), 8.48 (2H, d, J=9 Hz), 8.23 (2H, d, J=9 Hz), 8.12 (2H, d, J=9 Hz), 7.98 (1H, d, J=6 Hz), 7.44 (2H, d, J=9 Hz), 3.02 (1H, heptet, J=7 Hz), 1.33 (6H, d, J=7 Hz). MS (ES+): m/e 320 (20), 319 (100). MS (ES−): m/e 318 (20), 317 (100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09315467B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-aa838647d13644f78a6272a43cf00cc9 |
| Source note | uspto-grants-2016_04 |