HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 25260201, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 25259506 | HCID 25259506 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 25260201 | HCID 25260201 | 97% |
Reaction Steps
To a solution of Example 39A (4.26 g, 12.55 mmol) in 1,4-dioxane (15 mL) was added 4M sulfuric acid (15 mL) and the reaction was stirred at reflux for 48 hours. The solution was concentrated in vacuo and partitioned between water and methylene chloride. The methylene chloride layer was dried with sodium sulfate, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel eluting with hexane, 10% ethyl acetate in hexane, and 20% ethyl acetate in hexane to give the title compound (2.70 g, 97%). 1H NMR (300 MHz, CDCl3): δ ppm 0.88 (m, 6 H) 1.09 (m, 2 H) 1.52 (m, 4 H) 1.99 (m, 2 H) 7.35 (m, 5 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07538105B2 |
| Source dataset | uspto-grants-2009_05 |
| ORD ID | ord-ee08907e40b64bc89d6ce8cdc7402759 |
| Source note | uspto-grants-2009_05 |