Reaktionsgleichung
[Cl-].[NH4+].[Cl:3][C:4]1[CH:16]=[C:15]([N+:17]([O-])=O)[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1>[Zn]>[ClH:3].[Cl:3][C:4]1[CH:16]=[C:15]([NH2:17])[CH:14]=[CH:13][C:5]=1[NH:6][CH2:7][CH:8]1[O:12][CH2:11][CH2:10][CH2:9]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
3.0 g of ammonium chloride and 50 g of zinc powder are added to 150 ml of an aqueous-alcoholic solution (85% of alcohol and 15% of water). This mixture is heated to the reflux temperature, whilst stirring, and 0.1 mol (25.7 g) of 2-chloro-4-nitro-N-tetrahydrofurfurylaniline is then added gradually. When the addition has ended and the reaction mixture is decolorised, the latter is filtered and the filtrate is collected in 20 ml of ice-cooled hydrochloric acid. After cooling, the expected hydrochloride precipitates in the form of crystals. It is filtered off, washed with a small amount of ice-cooled absolute alcohol and dried in vacuo. It melts at about 170° C. with decomposition.
Aufarbeitung
- temperatureThis mixture is heated to the reflux temperature
- additionWhen the addition
- filtrationthe latter is filtered
- customthe filtrate is collected in 20 ml of ice-
- temperaturecooled hydrochloric acid
- temperatureAfter cooling
- customthe expected hydrochloride precipitates in the form of crystals
- filtrationIt is filtered off
- washwashed with a small amount of ice-
- temperaturecooled absolute alcohol
- customdried in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-7b37cd148ced4afebf90ae56e028634c
- Quelldatensatz
- uspto-grants-1979_04
- Patentnummer
- US04149848
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