HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 3-(3,4-dimethoxybenzyl)-7-fluoro-6-hydroxy-1-(tetrahydro-2H-pyran-4-yl)quinazoline-2,4(1H,3H)-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Ammonium formate | HCID 2723923 | — |
| Reactant | 6-(benzyloxy)-3-(3,4-dimethoxybenzyl)-7-fluoro-1-(tetrahydro-2H-pyran-4-yl)quinazoline-2,4(1H,3H)-dione | HCID 66732531 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 3-(3,4-dimethoxybenzyl)-7-fluoro-6-hydroxy-1-(tetrahydro-2H-pyran-4-yl)quinazoline-2,4(1H,3H)-dione | HCID 49764919 | 66.5% |
Reaction Steps
A mixture of 0.2 g of the compound obtained in Step 4.6, 0.036 g of ammonium formate and 0.041 g of Pd/C (10%) in 4 ml of EtOH is irradiated in a microwave field for 5 minutes at 60° C. DCM is added, the mixture is filtered and the filtrate is evaporated under reduced pressure. The residue is chromatographed on silica gel, eluting with a PE/EtOAc mixture from (95/5, v/v) to (0/100, v/v) to give 0.11 g of the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08722659B2 |
| Source dataset | uspto-grants-2014_05 |
| ORD ID | ord-7c03f8896d40420f9b0587273c793bac |
| Source note | uspto-grants-2014_05 |