HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Lutidine → HCID 22030256, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Lutidine | HCID 7937 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 135682056 | HCID 135682056 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 22030256 | HCID 22030256 | — |
Reaction Steps
Reflux a mixture of 7-(3-chloro-pyridin-2-yl)-2-methoxymethyl-3H-pyrido[2,3-d]pyrimidin-4-one (0.25 g), 2,6-lutidine (0.44 g), and POCl3 (0.51 g) in CHCl3 (5 mL) for 20 hours. Cool the mixture and concentrate under reduced pressure. Partition the residue between EtOAc and saturated NaHCO3 solution. Wash the EtOAc portion with additional NaHCO3 and then dry (Na2SO4) and concentrate under reduced pressure. Filter the brown residue through 2 inches of silica gel (1:1 EtOAc/hexanes eluent) and concentrate under reduced pressure to give 4-chloro-7-(3-chloro-pyridin-2-yl)-2-methoxymethyl-pyrido[2,3-d]pyrimidine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07304059B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-45bdfab4cb8e407ea533561750d40828 |
| Source note | uspto-grants-2007_12 |