Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Reactant | HCID 22273591 | HCID 22273591 | — |
| Reactant | 2-Oxopropanal methylhydrazone | HCID 72770268 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67050219 | HCID 67050219 | 5% |
Reaction Steps
2-Oxopropanal methylhydrazone (10.56 mmol, 1.06 g) and (3-bromo-4-fluorophenyl)(oxo)acetaldehyde (10.56 mmol, 2.44 g) synthesized in Reference Synthetic Example 9 were dissolved in acetic acid (37 mL) and stirred at 100° C. for 4.5 hours. Then, the solvent was evaporated, and the residue was dried by means of a vacuum pump and purified by silica gel column chromatography (n-hexane/ethyl acetate=3/1) then by silica gel thin layer chromatography (chloroform) and by silica gel thin layer chromatography (n-hexane/ethyl acetate=3/1) to give the desired product as a brown solid (160 mg, yield 5%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07576115B2 |
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| Source dataset | uspto-grants-2009_08 |
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| ORD ID | ord-2b58f808e7304226b159a20fc9841aeb |
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| Source note | uspto-grants-2009_08 |
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