Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | 1,4-Dioxa-8-thiaspiro(4.5)decane | HCID 12335978 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 65973-24-2 | HCID 13273782 | — |
Reaction Steps
A room temperature mixture of 13.8 g of product from Example 392 dissolved in 100 ml of acetic acid is treated, dropwise over 20 minutes, with 9.0 ml of 30% hydrogen peroxide. The reaction mixture is stirred at room temperature for 1 hour, concentrated in vacuo at 50° C., and extracted with ethyl acetate. The organic layer is washed 2× with saturated sodium bicarbonate, water and saturated sodium chloride, dried and concentrated in vacuo. The aqueous washes are combined and concentrated in vacuo to about 25 ml. The residue is saturated with solid potassium carbonate and extracted 2× with 200 ml of ethyl acetate. The organic phase is concentrated in vacuo to a solid which is triturated with hexane and collected to give 13.1 g of the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05750735 |
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| Source dataset | uspto-grants-1998_05 |
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| ORD ID | ord-78f0c7a9ea9e4c4a93abf5a8515edee3 |
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| Source note | uspto-grants-1998_05 |
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