HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorine → HCID 178427972, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorine | HCID 24526 | — |
| Reactant | HCID 178431875 | HCID 178431875 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 178427972 | HCID 178427972 | 82% |
Reaction Steps
To a solution of 5-methylthieno[2,3-d]pyrimidin-4-ol (2 g, 12 mmol) in acetic acid (30 mL) at room temperature, chlorine gas was bubbled for 3 h. The reaction mixture was stirred at same temperature for 2 days. The solvent was evaporated under reduced pressure at 40° C. and the residue was dissolved in ethyl acetate (30 mL) and washed with sat. NaHCO3 solution (3×20 mL). The organic layer was dried over sodium sulfate and evaporated to get the title compound as a pale yellow solid (2 g, 82%). 1H NMR (400 MHz, CDCl3 and CD3OD): δ 7.90 (s, 1H), 2.55 (s, 3H). MS (ESI) m/z: Calculated: 200.65; Observed: 201.3 (M++1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07612078B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-9c2431da5aa841eea6a1a216d6e3800b |
| Source note | uspto-grants-2009_11 |