Reaktionsgleichung
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([NH:9][NH2:10])=[O:8])=[CH:5][CH:4]=1.[C:13](Cl)(=[O:15])[CH3:14]>C1COCC1>[C:13]([NH:10][NH:9][C:7](=[O:8])[C:6]1[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=1)(=[O:15])[CH3:14]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To 40 mL of THF were added 1.8 g (10.8 mmol) of 4-methoxybenzoylhydrazine, 0.9 g (11.5 mmol) of acetyl chloride and 1.1 g of TEA. The reaction mixture was stirred for 1 hour, followed by evaporation off ca. ½ volume of THF. The product was precipitated into methanol, filtered and dried over night under vacuum. Yield was 2.14 g (95%). MS (EI, m/e) calcd for C10H12N2O3 208, found 208 M+, 6.7); mp 146-148° C.
Aufarbeitung
- customfollowed by evaporation off ca. ½ volume of THF
- customThe product was precipitated into methanol
- filtrationfiltered
- customdried over night under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-5372c1b158d64bbb9963923c5df5e946
- Quelldatensatz
- uspto-grants-2004_11
- Patentnummer
- US06815528B2
Verknüpfte Notizen
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