HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfide → HCID 59136009, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfide | HCID 1068 | — |
| Reactant | Triphenylphosphine Oxide | HCID 13097 | — |
| Reactant | Trifluoromethanesulfonic anhydride | HCID 67749 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 59135872 | HCID 59135872 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 59136009 | HCID 59136009 | 63% |
Reaction Steps
To a solution of triphenylphosphine oxide (1.98 g) in acetonitrile (30 mL) was slowly added trifluoromethanesulfonic anhydride (0.60 mL) at 0° C., and the mixture was stirred for 10 min. N-{[8-(Benzylthio)-1,4-dioxaspiro[4.5]dec-8-yl]methyl}-7-[methyl(2-thienylsulfonyl)amino]-1H-indole-2-carboxamide (1.45 g) and dimethylsulfide (0.52 mL) were added, and the reaction mixture was stirred at 0° C. for 30 min. Saturated aqueous sodium hydrogencarbonate was added, and the precipitated solid was collected by filtration, and washed with water. The obtained solid was washed with ethyl acetate, and dried to give the title compound (0.75 g, yield 63%) as colorless crystals. melting point 224-225° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652133B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-2d407e312386460690bf768a2b9764df |
| Source note | uspto-grants-2010_01 |