HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Ethoxycarbonyl-2-methylsulfinyl-4-oxo-4H-1-benzothiopyran → HCID 178418626, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Ethoxycarbonyl-2-methylsulfinyl-4-oxo-4H-1-benzothiopyran | HCID 19795759 | — |
| Reactant | Sodium hydrogen sulphide | HCID 86586439 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178418626 | HCID 178418626 | 23% |
Reaction Steps
To a solution of 100 mg (0.337 mmol) of the compound of Example 18 in 1.8 ml of tetrahydrofuran was added 1N sodium hydrogensulfide (0.697 mmol), and the mixture was stirred for 3 hours. Solvent was distilled off and 87 mg of sodium bicarbonate and 6.5 ml of water were added to the residue, which was washed with dichloromethane. After added 2.2 ml of 1N hydrochloric acid, this was extracted with dichloromethane. The organic layer was washed with saturated saline solution and concentrated. The residue was purified by means of silica gel column chromatography (CHCl3) to obtain title compound (yield 23%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05244892 |
| Source dataset | uspto-grants-1993_09 |
| ORD ID | ord-e4a23dd9d11840d1854afd3d74c6084e |
| Source note | uspto-grants-1993_09 |