Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | HCID 25241888 | HCID 25241888 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 57385684 | HCID 57385684 | — |
Reaction Steps
Compound (11a) is dissolved in an appropriate solvent, preferably in dimethylsulfoxide, and treated with a solution of IBX, preferably in dimethylsulfoxide. After stirring for up to several hours, water is added and the white precipitate is removed by filtration. The precipitate is washed, preferably with dimethylsulfoxide/water and a small amount of AcOEt. The filtrate is extracted, preferably with dichloromethane for several times, the combined organic phases are dried (using e.g. Na2SO4) and concentrated, preferably in vacuo. Chromatography purification (using e.g. a polar solvent gradient) is employed to yield compound (12a). The reaction of compound (11a) (A) and IBX (B) is preferably carried out with equivalents, on a molar basis, of A:B in the ratio of about 1:2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08809395B2 |
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| Source dataset | uspto-grants-2014_08 |
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| ORD ID | ord-dd0f1937a6164ca792ace36cdc9655c7 |
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| Source note | uspto-grants-2014_08 |
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