Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | 2-(2,4-difluorophenoxy)-2-methylpropanoic acid | HCID 1531801 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58243728 | HCID 58243728 | 69.8% |
Reaction Steps
HOBt (1.76 g) and WSC•monohydrochloride (2.49 g) were added to a solution of 2-(2,4-difluorophenoxy)-2-methylpropanoic acid (2.34 g) in acetonitrile (27 ml), followed by stirring at room temperature for one hour. This solution was added dropwise to a solution of hydrazine monohydrate (3.25 g) and triethylamine (3.0 ml) in acetonitrile (20 ml) under ice cooling, followed by stirring at room temperature for 2 hours, the reaction solution was concentrated under reduced pressure, and saturated aqueous sodium bicarbonate was added thereto, followed by extraction with chloroform. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=98:2) to obtain 2-(2,4-difluorophenoxy)-2-methylpropanohydrazide (1.74 g).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08377923B2 |
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| Source dataset | uspto-grants-2013_02 |
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| ORD ID | ord-d3ff1945a2d1415581c0edf84f74c947 |
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| Source note | uspto-grants-2013_02 |
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