HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → N-[2-methyl-3(2-oxo-ethyl)-phenyl]-methanesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | N-(3-cyanomethyl-2-methyl-phenyl)-methanesulfonamide | HCID 18789726 | — |
| Reactant | Diisobutylaluminumhydride | HCID 21225700 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-[2-methyl-3(2-oxo-ethyl)-phenyl]-methanesulfonamide | HCID 18789617 | — |
Reaction Conditions
| Temperature | 5 °C |
|---|
Reaction Steps
N-(3-cyanomethyl-2-methyl-phenyl)-methanesulfonamide (3.75 g) was dissolved in 50 ml of dry tetrahydrofuran and cooled in an ice bath under an atmosphere of nitrogen. To this mixture was added 67 ml of 1M diisobutylaluminum hydride (DIBAL) in tetrahydrofuran. The mixture was stirred at 5° C. for 75 minutes. Excess reagent was decomposed with methanol and the solvent was evaporated. The residue was treated with EtOAc, washed with cold 1M hydrochloric acid, washed with brine and dried, and the solvent was evaporated. The residue was purified by silica gel chromatography eluting with methanol:dichloromethane (5:95), giving 1.1 g of N-[2-methyl-3(2-oxo-ethyl)-phenyl]-methanesulfonamide as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05952362 |
| Source dataset | uspto-grants-1999_09 |
| ORD ID | ord-8b4f15751fb748c3952b89fe9c0187fe |
| Source note | uspto-grants-1999_09 |