HuagongsheHuagongshe Chemistry Print Report · For research reference only
tert-Butylsulfinamide, (R)-(+)- → (NE,R)-2-methyl-N-[1-(5-methylsulfonylfuran-2-yl)propylidene]propane-2-sulfinamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | tert-Butylsulfinamide, (R)-(+)- | HCID 10964479 | — |
| Reactant | 1-(5-Methanesulfonyl-furan-2-yl)-propan-1-one | HCID 59278141 | — |
| Catalyst | Titanium isopropoxide | HCID 11026 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (NE,R)-2-methyl-N-[1-(5-methylsulfonylfuran-2-yl)propylidene]propane-2-sulfinamide | HCID 59278140 | — |
Reaction Steps
To a solution of 1-(5-methanesulfonyl-furan-2-yl)-propan-1-one (1.1 g, 5.5 mmol) in THF (30 mL) was added (R)-(+)-2-methyl-2-propanesulfinamide (0.750 g, 6.06 mmol) and titanium (IV) isopropoxide (6 mL, 25 mmol) and the mixture was warmed at reflux. After 18 hours, the mixture was cooled to room temperature, and diluted with diethyl ether (100 mL) and water (6 mL). The mixture was stirred for 10 minutes, dried over sodium sulfate, filtered and concentrated. The crude product was purified by silica gel chromatography, eluting with a gradient of 0-80% EtOAc-hexanes to afford (R)-2-methyl-propane-2-sulfinic acid[1-(5-methanesulfonyl-furan-2-yl)-prop-(E)-ylidene]-amide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07879873B2 |
| Source dataset | uspto-grants-2011_02 |
| ORD ID | ord-20925c42e2b94c59bf47461a05c8c1bb |
| Source note | uspto-grants-2011_02 |