HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 7-Chloro-3-methylthieno(3,2-b)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 178431852 | HCID 178431852 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | 7-Chloro-3-methylthieno(3,2-b)pyridine | HCID 57415864 | 55.8% |
Reaction Steps
Phosphorous oxychloride (2.2 mL, 24 mmol) in 1,2-dichloroethane (12 mL) was charged with 3-methylthieno[3,2-b]pyridin-7-ol (2.0 g, 12 mmol). The reaction stirred overnight at reflux under nitrogen. The mixture was the cooled and concentrated. Saturated NaHCO3 solution was carefully added to neutralize the residue. The biphasic mixture was extracted with dichloromethane, dried, and concentrated. Flash chromatography (15% EtOAc/hexanes) gave the title compound (1.23 g, 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354540B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-7177100b147b459db6fb664eae1a6917 |
| Source note | uspto-grants-2013_01 |