HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 7-Bromo-4-chlorothieno[3,2-d]pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 7-Bromothieno(3,2-d)pyrimidin-4-ol | HCID 135743712 | — |
| Product | 7-Bromo-4-chlorothieno[3,2-d]pyrimidine | HCID 16655266 | 82% |
Reaction Steps
A solution of 7-bromo-3H-thieno[3,2-d]pyrimid-4-one (126, 0.94 g, 4.1 mmol) in phosphorus oxychloride (4 mL) under N2 was heated at reflux for 1 hour. The resulting solution was allowed to cool to room temperature and then poured into a saturated aqueous solution of sodium bicarbonate to neutralize. The aqueous mixture was extracted with ethyl acetate. The organic layer was washed with water followed by saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and the solvent evaporated under reduced pressure to yield 7-bromo-4-chlorothieno[3,2-d]pyrimidine (0.83 g, 82% yield) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07285556B2 |
| Source dataset | uspto-grants-2007_10 |
| ORD ID | ord-7e11a6e63a074865bc8947ca01261016 |
| Source note | uspto-grants-2007_10 |