HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium fluoride → HCID 22125153, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium fluoride | HCID 25516 | — |
| Reactant | HCID 54384838 | HCID 54384838 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22125153 | HCID 22125153 | 96% |
Reaction Steps
A solution of 400 mg (0.55 mmol) of 3-(2-bromophenyl)-1-[3-(tert-butyldiphenylsilyloxymethyl)phenyl]-3,4-dihydro-7-methanesulfonyl-pyrimido[4,5-d]pyrimidin-2(1H)-one in 30 ml of methanol was treated with 400 mg (11 mmol) of ammonium fluoride and the mixture heated at reflux for 1 hour. The mixture was evaporated and the product purified by flash chromatography on silica gel eluting with dichloromethane/methanol in a ratio of 20:1. The product-containing fractions were combined and evaporated to afford 257 mg (96%) of 3-(2-bromophenyl)-3,4-dihydro-1-[3-(hydroxymethyl)phenyl]-7-methanesulfonyl-pyrimido[4,5-d]pyrimidin-2(1H)-one as a white solid. [Mass spectrum (ESI) MH+ =490].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06150373 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-e7d7cc232e94420596f22d4ae10e954d |
| Source note | uspto-grants-2000_11 |