Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Butanoic acid, 2-(ethoxymethylene)-3-oxo-, ethyl ester | HCID 97734 | — |
| Reactant | 4-(Trifluoromethoxy)phenylhydrazine hydrochloride | HCID 2777328 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 10660835 | HCID 10660835 | 71.1% |
Reaction Steps
4-Trifluoromethoxyphenylhydrazine hydrochloride (4.0 g) and ethyl 2-ethoxymethylene-acetoacetate (3.26 g) prepared according to a method described in J. Chem. Soc. Perkin trans. I, 1875 (1988), were added to a mixed solvent of water (10 ml) and ethanol (10 ml), and stirred at 76° C. for two hours. Sodium hydroxide (1.40 g) was added to the reaction solution and the mixture was further stirred at the same temperature for an hour. Ethanol was evaporated in vacuo, hydrochloric acid (1 mole/1) was added to the aqueous solution and the precipitated solid was recrystallized from ethyl acetate to give the titled compound (3.56 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09150555B2 |
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| Source dataset | uspto-grants-2015_10 |
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| ORD ID | ord-ab84c198e7a54e5db4b229309cbde668 |
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| Source note | uspto-grants-2015_10 |
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