HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methylamine → HCID 22125000, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 22125008 | HCID 22125008 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 22125000 | HCID 22125000 | 16% |
Reaction Steps
A solution of 120 mg (0.2 mmol) of 7-anilino-3-(2,4-dichlorophenyl)-3,4-dihydro-1-[3-(2-methanesulfonyloxyethyl)phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one in 4 ml of 40% methylamine in ethanol was heated at 50° C. for 3 hours. The reaction mixture was evaporated and the crude material purified by flash column chromatography on silica gel eluting with dichloromethane/methanol/acetic acid/water (120:14:3:2). Product containing fractions were combined and evaporated to give 18 mg (16%) of 7-anilino-3-(2,4-dichlorophenyl)-3,4-dihydro-1-[3-[2-(methylamino)ethyl]phenyl]pyrimido[4,5-d]pyrimidin-2(1H)-one as a solid of melting point 120-122° C. [Mass spectrum (ESI) MH+ =519].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06150373 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-50c4b82f9243419f875cf6e5ae317ee1 |
| Source note | uspto-grants-2000_11 |