HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 22030341, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 135682064 | HCID 135682064 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 22030341 | HCID 22030341 | — |
Reaction Steps
Dissolve 7-(3-trifluoromethyl-pyridin-2-yl)-2-methoxymethyl-3H-pyrido[3,2-d]pyrimidin-4-one (276 mg, 0.822 mmol) in CHCl3 (25 mL) and 2,6-lutidine (294 mg, 2.74 mmol). Add phosphorous oxycloride (0.255 mL, 2.74 mmol) dropwise and heat the resulting solution to reflux for 24 hours. Cool the solution and remove the solvent under reduced pressure. Partition the crude residue between EtOAc (50 mL) and saturated NaHCO3 (aq) (50 mL). Remove the organic phase and extract the aqueous phase with additional EtOAc (50 mL). Combine the two organic extracts, wash with brine (100 mL), and dry over Na2SO4. Remove the solvent to yield the title compound as a light brown solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07304059B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-0b1c0c215e0a40efbeb801db3dfb83a9 |
| Source note | uspto-grants-2007_12 |