HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 71612269, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 71612022 | HCID 71612022 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 71612269 | HCID 71612269 | 87% |
Reaction Steps
To a solution of 722 mg of ethyl 4-({2-[5-cyclopropyl-1-(4-ethoxy-2,6-difluorobenzyl)-4-methyl-1H-pyrazol-3-yl]-5-methoxypyrimidin-4-yl}amino)-pyridine-3-carboxylate 2-6-5 (1.28 mmol, 1.0 eq) in 13 mL THF and 1.6 mL methanol were added 256 mg sodium hydroxide (6.39 mmol, 5.0 eq). The mixture was stirred for 45 minutes at rt. Using 10% aqueous citric acid the pH of the mixture was adjusted to 3.5. The resulting suspension was filtered. The precipitate was washed with water and ethanol and subsequently dried to provide 660 mg of the desired product (1.11 mmol, 87%) as 90% pure target compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09422268B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-0823625d10e548f18e5476fc5ab3bd2d |
| Source note | uspto-grants-2016_08 |