HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzenesulfonyl chloride → 4-[[4-Methoxybenzenesulfonyl]amino]-4-carbomethoxy-tetrahydrothiopyran
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methyl 4-aminothiane-4-carboxylate hydrochloride | HCID 22907152 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[[4-Methoxybenzenesulfonyl]amino]-4-carbomethoxy-tetrahydrothiopyran | HCID 22907082 | — |
Reaction Steps
To a solution of 4-amino-4-carbomethoxy-tetrahydrothiopyran hydrochloride (3.1 g, 15.0 mmol) in methylene chloride (75 mL) containing triethylamine (3.5 g, 330.0 mmol) is added 4-methoxybenzenesulfonyl chloride (4.1 g, 20.0 mmol) at room temperature. The reaction mixture is stirred at room temperature for 18 hours. The mixture is diluted with water and the organic layer is removed. The aqueous layer is extracted with diethyl ether and the organic extracts are washed with brine, dried (MgSO4) and the solvent is evaporated. The product is purified by silica gel chromatography (50% ethylacetate/hexanes) to provide 4-[[4-methoxybenzenesulfonyl]amino]-4-carbomethoxy-tetrahydrothiopyran.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05506242 |
| Source dataset | uspto-grants-1996_04 |
| ORD ID | ord-5d29c42325464e6b8986adedbd7e81c6 |
| Source note | uspto-grants-1996_04 |