HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → 1-[2,6-Dichloropyrimidin-4-yl]-5-[2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl]-2,4(1H,3H)-pyrimidinedione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,4,6-Trichloropyrimidine | HCID 77378 | — |
| Reactant | 5-(2,8-Dimethyl-5h-dibenzo[a,d]cyclohepten-5-yl)-2,4(1h,3h)-pyrimidinedione | HCID 22117213 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | 1-[2,6-Dichloropyrimidin-4-yl]-5-[2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-yl]-2,4(1H,3H)-pyrimidinedione | HCID 18689772 | — |
Reaction Steps
Cesium carbonate (5 g) was added to a solution of the product of example 8 step (i) (5 g) in 1-methyl-2-pyrrolidinone (50 ml). After 5 minutes 2,4,6-trichloropyrimidine (2.8 g) was added. After 2 hours the reaction was partitioned between brine and ethyl acetate. The organic phase was washed with water, dried (MgSO4) and evaporated under reduced pressure. Purification was by chromatography eluting with 30% ethyl acetate in toluene. Yield 2.9 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06107297 |
| Source dataset | uspto-grants-2000_08 |
| ORD ID | ord-848f047d93254a34847dfc85bc912591 |
| Source note | uspto-grants-2000_08 |