Reaktionsgleichung
Cl.[NH2:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH3:10])=[C:5]([Cl:11])[C:4]=1[OH:12].C(N(CC)C1C=CC=CC=1)C.[CH3:24][C:25](C)=[O:26].C(Cl)(=O)C>O>[C:25]([NH:2][C:3]1[CH:8]=[C:7]([Cl:9])[C:6]([CH3:10])=[C:5]([Cl:11])[C:4]=1[OH:12])(=[O:26])[CH3:24]Komponenten
6
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a mixture of 68.4 g. of 2-amino-5-methyl-4,6-dichloro-phenol hydrochloride and 96 ml. of N,N-diethylaniline in 750 ml. of acetone, 23.4 ml. of acetyl chloride were added slowly by keeping the temperature under 20° C. At the end, the reaction mixture was heated to reflux for an hour. After cooling, the solution was poured into water; the solid product, thus obtained, was collected on a buckner, washed with water until the washings were neutral and dried in a desicator at 50° C. The raw product obtained was purified by crystallization from ethyl alcohol, yielding 44 g. of a pure product with M.P. = 175°-176.5° C.
Aufarbeitung
- additionTo a mixture of 68.4 g
- customunder 20° C
- temperatureAt the end, the reaction mixture was heated
- temperatureto reflux for an hour
- temperatureAfter cooling
- customthe solid product, thus obtained
- customwas collected on a buckner
- washwashed with water until the washings
- customdried in a desicator at 50° C
Quellen und Nachweise
- ORD-Eintrag
- ord-276cb44cd9e64c2f9dbd148d277632b1
- Quelldatensatz
- uspto-grants-1978_08
- Patentnummer
- US04110116
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