Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | Nitromethane | HCID 6375 | — |
| Edukt | Ammonium Acetate | HCID 517165 | — |
| Edukt | 4-(5-Methyl-pyridin-2-yloxymethyl)-benzaldehyde | HCID 59255142 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 59255428 | HCID 59255428 | 100,4% |
Reaktionsschritte
To an acetic acid (20.0 mL) solution of 4-(5-methyl-pyridin-2-yloxymethyl)-benzaldehyde (2.93 g, 12.9 mmol) described in Manufacturing Example 44-1-2 were added nitromethane (3.94 g, 64.5 mmol) and ammonium acetate (1.99 g, 25.8 mmol) under nitrogen atmosphere at room temperature, which was stirred for 2.5 hours at 100° C. Water and ethyl acetate were added to the reaction mixture, and the organic layer was extracted with ethyl acetate. This organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (3.50 g) as a crude product.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08153662B2 |
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| Quelldatensatz | uspto-grants-2012_04 |
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| ORD ID | ord-9b87b5a91f3c4448a96b1df4949990e0 |
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| Quellennotiz | uspto-grants-2012_04 |
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