HuagongsheHuagongshe Chemistry Print Report · For research reference only
6-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione → HCID 19045534, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 6-Chloro-1,3-dimethyl-2,4(1H,3H)-pyrimidinedione | HCID 81442 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 45158372 | HCID 45158372 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 19045534 | HCID 19045534 | 61% |
Reaction Steps
A solution of 3,4-dihydro-6-methoxyspiro[(2H)-1-benzopyran-2,4'-piperidin]-4-one hydrochloride (0.568 g, 2 mmol), 6-chloro-1,3-dimethylpyrimidine-2,4-(1H,3H)-dione (0.349 g, 2 mmol) and sodium bicarbonate (0.42 g, 5 mmol) in acetonitrile was heated at reflux for 42 hours. After cooling, the reaction mixture was concentrated in vacuo to dryness. The residue was partitioned between chloroform and water. The chloroform solution was washed twice with water and once with saturated brine solution and then dried over sodium sulfate and concentrated to dryness in vacuo. The solid residue was recrystallized from methanol/ethanol to give the title compound (0.47 g, 61% yield) mp 202°-203° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05633247 |
| Source dataset | uspto-grants-1997_05 |
| ORD ID | ord-5316fdb95ac1472fad8e43ff4c6050cf |
| Source note | uspto-grants-1997_05 |