HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetic Acid → HCID 12904736, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetic Acid | HCID 300 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 12904727 | HCID 12904727 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 12904736 | HCID 12904736 | — |
Reaction Steps
A suspension of 3.0 g of 6-(2,6-dichlorophenyl)-2-methylpyrido[2,3-d]pyrimidin-7-amine and 50 ml of 1,2-dichloroethane is boiled on a steam bath until the distilling vapors reach a temperature of 83° C. The suspension is cooled to room temperature and 1.6 g of chloroacetic acid and 2.6 g of carbonyldiimidazole are added sequentially. The mixture is stirred at room temperature for 3 hours and the resulting solution is immediately chromatographed over 150 g of silica gel. The crude product is eluted with a 99/1 chloroform/methanol mixture. Trituration of this with ether gives pure 2-chloro-N-[6-(2,6-dichlorophenyl)-2-methylpyrido[2,3-d]-pyrimidin-7-yl]acetamide, decomposing above ca 170° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04271164 |
| Source dataset | uspto-grants-1981_06 |
| ORD ID | ord-99e07c292fd446439dcd4be3ec25d0d1 |
| Source note | uspto-grants-1981_06 |