HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 54210792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | HCID 22125008 | HCID 22125008 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 54210792 | HCID 54210792 | 28% |
Reaction Steps
A solution of 58 mg (0.1 mmol) of 7-anilino-3-(2,4-dichlorophenyl)-3,4-dihydro-1-[3-(2-methanesulfonyloxyethyl)phenyl]-pyrimido[4,5-d]pyrimidin-2(1H)-one (prepared in Example 74) and 0.5 ml of diethylamine in 2 ml of ethanol was heated at 50° C. for 3 hours. The reaction mixture was evaporated and the crude material purified by flash chromatography on silica gel, eluting with 5% methanol in dichloromethane. Product containing fractions were combined and evaporated to give 16 mg (28%) of 7-anilino-3-(2,4-dichlorophenyl)-1-[3-[2-(diethylamino) ethyl]phenyl]-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one as an off-white solid of melting point 186° C. [Mass spectrum (ESI) MH+ =561].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06150373 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-cc585e36dd574486a3e45fa0ef1acaf4 |
| Source note | uspto-grants-2000_11 |