HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(2,5,5-Trimethyl-1,3-dioxan-2-yl)thiophene-2-sulfonamide → 3-Acetyl-2-thiophenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(2,5,5-Trimethyl-1,3-dioxan-2-yl)thiophene-2-sulfonamide | HCID 22901938 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 3-Acetyl-2-thiophenesulfonamide | HCID 22901926 | 79% |
Reaction Steps
The product from Step A (174.05 g, crude) was dissolved in a mixture of THF (1000 mL) and 1N HCl (1000 mL) and heated at reflux temperature for 1.5 hr. The THF was evaporated and the aqueous solution made basic by the addition of a saturated aqueous sodium bicarbonate solution. The mixture was cooled and the precipitate collected by filtration, washed with cold water and dried in vacuo to give the crude product (109.1 g,). Recrystallization from acetonitrile gave the desired product (81.5 g, 79%): mp 193°-196° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05538966 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-a3f062ca59674ecb9fa508a3b1bad15d |
| Source note | uspto-grants-1996_07 |