Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Sodium periodate | HCID 23667635 | — |
| Reactant | HCID 59025495 | HCID 59025495 | — |
| Catalyst | Ruthenium trichloride hydrate | HCID 6093376 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 59025536 | HCID 59025536 | — |
Reaction Steps
701.6 mg of sodium periodate (3.28 mol) and 3.6 mg of ruthenium(III) chloride monohydrate (0.02 mol) are introduced into 3 ml of water. 229.4 mg of the compound from Example 24A (0.80 mol) dissolved in 2 ml of tetrachloromethane are added and, after addition of 2 ml of acetonitrile, the reaction mixture is stirred at room temperature for 16 h. For working up, the mixture is poured into 20 ml of a 5% strength aqueous trifluoroacetic acid solution and extracted three times with dichloromethane. The combined organic phases are dried over sodium sulphate, and the solvent is removed in a rotary evaporator. The residue is stirred with 5 ml of ethyl acetate and 2 ml of n-heptane and stored at 5° C. for 3 h. The deposited product is filtered off, washed with m-pentane and dried under high vacuum. 119.0 mg (44% of theory) of the title compound are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07662956B2 |
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| Source dataset | uspto-grants-2010_02 |
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| ORD ID | ord-d4acfe09f1914db1a8dd070486357c0e |
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| Source note | uspto-grants-2010_02 |
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