HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Thieno(2,3-c)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | N-(2,2-dimethoxyethyl)-4-methyl-N-(thiophen-2-ylmethyl)benzenesulfonamide | HCID 334477 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | Thieno(2,3-c)pyridine | HCID 9224 | — |
Reaction Steps
N-(2,2-Dimethoxyethyl)-4-methyl-N-(thiophen-2-ylmethyl)benzenesulfonamide (7 g, 19 mmol) was dissolved in dioxane (10 mL) and treated with concentrated HCl (10 mL). The mixture for heated to reflux for 12 h. The mixture was allowed to cool down to room temperature, diluted with water (20 mL) and brought to pH 7 with 2 N sodium hydroxide. The mixture was then extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate, water and brine. The organic layer was dried with sodium sulfate, concentrated and purified by flash chromatography using a gradient of 10 to 60% ethyl acetate in hexanes to obtain a tan solid. Yield=1 g. MS (M+H)+ 136.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07786132B2 |
| Source dataset | uspto-grants-2010_08 |
| ORD ID | ord-50bb974d256a4ddd956df49c78c11e41 |
| Source note | uspto-grants-2010_08 |