HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → 2-(3-Chlorophenyl)-2-(4,6-dimethoxypyrimidin-2-yl)propiononitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (3-Chlorophenyl)(4,6-dimethoxypyrimidin-2-yl)acetonitrile | HCID 19882861 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 2-(3-Chlorophenyl)-2-(4,6-dimethoxypyrimidin-2-yl)propiononitrile | HCID 19882857 | 62% |
Reaction Steps
Sodium hydride (0.83 g of 80% in oil) was added to a stirred solution of the product of Example 48 (8.0 g) in dimethylformamide at room temperature. Dimethyl sulphate (3.5 g) was then added, and the mixture was stirred at room temperature for 4 hours. The mixture was poured onto water (250 ml), and the oil was extracted into ethyl acetate. The combined extracts were dried over magnesium sulphate, and evaporated to give an orange liquid, which was purified by chromatography to give 5.2 g of the desired product as a white solid, mp 89°-93° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05137564 |
| Source dataset | uspto-grants-1992_08 |
| ORD ID | ord-21ba1516c79949f5af8729f196399fdc |
| Source note | uspto-grants-1992_08 |