Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | HCID 18645506 | HCID 18645506 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 18645505 | HCID 18645505 | — |
Reaction Steps
Trans-4-(2-acetylhydrazino)-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-3-ol, 320 mg, was dissolved in 6 ml of chloroform and to this was added 0.5 ml of pyridine. While stirring under water cooling (20° C.), 0.23 ml of acetyl chloride was added and the mixture was stirred at room temperature for 3 hours. The solvent was distilled off under a reduced pressure, and to the residue was added ice water to scrape and crush it. After filtration and drying, it was recrystallized from ethyl acetate - hexane (1:1) to give 260 mg of trans-4-(1,2-diacetylhydrazino)-6-cyano-3,4-dihydro-2,2-dimethyl-2H-1-benzopyran-3-ol as white crystals, m.p. 230°-233° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05318969 |
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| Source dataset | uspto-grants-1994_06 |
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| ORD ID | ord-9ba1da46f37e46e8983d8fea3c6a0129 |
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| Source note | uspto-grants-1994_06 |
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