HuagongsheHuagongshe Chemistry Print Report · For research reference only
(+/-)-5-(9,10-Dihydro-4-hydroxy-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione → HCID 70112978, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (+/-)-5-(9,10-Dihydro-4-hydroxy-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione | HCID 70113472 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 70112978 | HCID 70112978 | — |
Reaction Steps
A stirred solution of the product from step (ii) (280 mg) in trifluoroacetic acid (5 ml), was heated under reflux for 96 h and evaporated. The residue was slurried in toluene and evaporated (twice). Purification was by flash chromatography eluting 50% acetone in isohexane, followed by a second column eluting with 4% ethanol in dichloromethane to give a yellow solid. Yield 75 mg. Used directly in the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06218376B1 |
| Source dataset | uspto-grants-2001_04 |
| ORD ID | ord-b488002cf17345908f01d8d9891489b6 |
| Source note | uspto-grants-2001_04 |