HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 6-Bromo-3-methyl-4-pyridin-2-yl-3,4-dihydro-1H-quinazolin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | 4-Bromo-2-(methylamino-pyridin-2-yl-methyl)-phenylamine | HCID 117600061 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 6-Bromo-3-methyl-4-pyridin-2-yl-3,4-dihydro-1H-quinazolin-2-one | HCID 117600626 | — |
Reaction Steps
To a solution of crude 4-Bromo-2-(methylamino-pyridin-2-yl-methyl)-phenylamine (500 mg) in THF (20 mL) is added triphosgene (493 mg, 1.87 mmol), then the mixture is stirred at room temperature for 2 h. TLC showed the reaction is completed. Water (20 mL) is added and the mixture is extracted with EtOAc, the organic layer is dried over Na2SO4 and concentrated to give the desired compound as a crude mixture. This is used in next step with no further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09199988B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-4ebc16553abd4488950a5bef1ee3aef4 |
| Source note | uspto-grants-2015_12 |