Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Butyryl chloride | HCID 8855 | — |
| Reactant | HCID 178463101 | HCID 178463101 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 18348345 | HCID 18348345 | — |
Reaction Steps
1.5 g (3.9 mmol) of 1-ethyl-5-hydroxy-4-(8-methyl-2,3-dihydro-1,1,4,4-tetraoxobenz[1,4]dithiin-7-yl)carbonylpyrazole were suspended in 20 ml of methylene chloride, and 0.42 g (3.9 mmol) of butyryl chloride and 0.39 g (0.42 mol) of triethylamine were added. After five hours of stirring at 20° C., the mixture was washed with 2N hydrochloric acid, sodium bicarbonate solution and water, dried and filtered off, and the solvent was distilled off. The residue was subsequently chromatographed over silica gel (mobile phase: ethyl acetate/cyclohexane=2/3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06326333B1 |
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| Source dataset | uspto-grants-2001_12 |
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| ORD ID | ord-52057da94476481d85af72206603405d |
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| Source note | uspto-grants-2001_12 |
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