HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 21104300, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 136008001 | HCID 136008001 | — |
| Product | HCID 21104300 | HCID 21104300 | 55% |
Reaction Steps
1-Butyl-6-(2-fluoro-phenyl)-3-methyl-1,5-dihydro-pyrazolo[3,4-d]pyrimidin-4-one (1.23 g, 4.1 mmole) was dissolved in phosphorous oxychloride (15 ml) and heated to reflux overnight. The excess phosphorous oxychloride was removed under vacuum, the residue was treated with ice water, the product was extracted into ethyl acetate, washed with water, saturated sodium chloride, then dried over sodium sulfate (anh.) and the solvent was removed to give the crude product. The product was chromatographed on silica gel eluting with chloroform to give 723 mg of purified product (yield: 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07977342B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-924fc7f83ee74ab384a105432dfee770 |
| Source note | uspto-grants-2011_07 |