HuagongsheHuagongshe Chemistry Print Report · For research reference only
(2-Chlorophenyl)-(4,6-dichloro-2-methylsulfanylpyrimidin-5-yl)-methanol → (2-Chlorophenyl)-(4,6-dichloro-2-methylsulfanylpyrimidin-5-yl)-methanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (2-Chlorophenyl)-(4,6-dichloro-2-methylsulfanylpyrimidin-5-yl)-methanol | HCID 59812918 | — |
| Catalyst | HCID 178418406 | HCID 178418406 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | (2-Chlorophenyl)-(4,6-dichloro-2-methylsulfanylpyrimidin-5-yl)-methanone | HCID 59812853 | 16.3% |
Reaction Steps
To a solution of (2-chlorophenyl)-(4,6-dichloro-2-methylsulfanylpyrimidin-5-yl)-methanol (8.6 g, 25.6 mmol) in toluene (300 mL) was added manganese (IV) oxide (Aldrich) (22.3 g, 10 eq), and the resulting mixture was heated to reflux with stirring for a total of 5 hours. The reaction was cooled to room temperature and then filtered through a 3.5 cm pad of Celite and the filtrate was concentrated to give 8.84 g of a crude product. Purification by Flash Column Chromatography on Silica Gel eluting with a gradient starting with pure hexanes and progressing to 2% ethyl acetate in hexanes and finally 5% ethyl acetate in hexanes gave the title compound as an off-white powder (1.388 g, (M+H)+=333).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07566708B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-e3264fae951c42d89289ea608f80d909 |
| Source note | uspto-grants-2009_07 |