Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrogen Peroxide | HCID 784 | — |
| Reactant | HCID 22118438 | HCID 22118438 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22118408 | HCID 22118408 | 97% |
Reaction Steps
A 100-ml round-bottomed flask was charged with 1.18 g (4.50 mmol) of 6-acetyl-3,3,5,8-tetramethylthiochroman-4-one, 2 ml of acetic acid and 1.12 g (9.88 mmol) of a 30 wt % hydrogen peroxide aqueous solution, and the mixture was allowed to react at 80° C. for 2 and half hours. The reaction mixture was diluted with about 30 ml of water, and a sodium hydrogensulfite aqueous solution was added to decompose excess peroxide. Then, the mixture was extracted with ethyl acetate. An organic layer was washed with a saturated sodium hydrogencarbonate aqueous solution and with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure to give 1.28 g (yield 97%) of 6-acetyl-3,3,5,8-tetramethylthiochroman-4-one-1,1-dioxide.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06159904 |
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| Source dataset | uspto-grants-2000_12 |
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| ORD ID | ord-6fbfa37d1e194014900a6a29686abb86 |
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| Source note | uspto-grants-2000_12 |
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