HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → HCID 25068477, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| Reactant | Cornforth reagent | HCID 2724130 | — |
| Reactant | HCID 15816085 | HCID 15816085 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 25068477 | HCID 25068477 | 92.1% |
Reaction Steps
The compound of Example 8F (70 mg, 0.25 mmol) was dissolved in 1.5 mL of dichloromethane; 350 mg of pyridinium dichromate and 15 mg of pyridinium p-toluenesulfonate were added, and the resultant mixture was stirred overnight at ambient temperature. Solvents were removed in vacuo; the residue was taken up in ethyl acetate and filtered through diatomaceous earth washing with ethyl acetate. The filtrate was concentrated and the residue was purified by chromatography on an Analogix Intelliflash 280™, eluting with a gradient of 10% to 40% ethyl acetate in hexanes, to isolate the titled compound (65 mg, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08377913B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-b44c0c159f7d493199e17d638c75b712 |
| Source note | uspto-grants-2013_02 |