HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 4-Chloro-2-(5-chloro-2-thienyl)-5-ethyl-6-methyl-pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 2-(5-chloro-2-thienyl)-5-ethyl-4-methyl-1H-pyrimidin-6-one | HCID 135996612 | — |
| Product | 4-Chloro-2-(5-chloro-2-thienyl)-5-ethyl-6-methyl-pyrimidine | HCID 61000230 | 66% |
Reaction Steps
An 100-mL round bottomed flask was charged 2-(5-Chloro-2-thienyl)-5-ethyl-4-methyl-1H-pyrimidin-6-one (4 g, 15.7 mmol). POCl3 (16 ml) was added. The resulting mixture was stirred at 90 C for 6 hr. After cooling to room temperature, the volatile material was removed under reduced pressure and the residue was with NaHCO3 aq (100 ml). Dichloromethane was added. The organic layer was separated and passed through a plug of silica gel, using dichloromethane as eluent to give the title compound as a solid (2.82 g, 66% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221843B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-8000bc6ad3044a4bbd0a80893652f68f |
| Source note | uspto-grants-2015_12 |