HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Chloro-2(1H)-pyrimidinone → HCID 12795547, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Chloro-2(1H)-pyrimidinone | HCID 108578 | — |
| Reactant | 2-Chloro-4'-fluoroacetophenone | HCID 120248 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 12795547 | HCID 12795547 | 7.6% |
Reaction Steps
A solution of 5-chloropyrimidin-2-one (1.309 g) and 2-chloro-4'-fluoroacetophenone (1.726 g) in triethylamine (2 ml) and ethanol (50 ml) was stirred and heated at reflux for 11/2 hours. After evaporation of solvents, the residue was triturated with water (100 ml). The resulting collected solid was crystallised from ethanol then acetone, but still required purification, by preparative thin-layer chromatography on silica developed in chloroform-ethanol (25:1 v/v), before crystallisation from propan-2-ol to give the title pyrimidinone (204 mg,); 196°-202°; λmaxEtOH 245 nm (ε 17780), 333 nm (ε 2090), λinf 236 nm (ε 15230), 280 nm (ε 980).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04636509 |
| Source dataset | uspto-grants-1987_01 |
| ORD ID | ord-bbc6afbfa8e746e5bc0647d12016a524 |
| Source note | uspto-grants-1987_01 |