Reaktion #54620

Reaktionsgleichung

ammonium chloride

2-chloro-4-nitro-N-tetrahydrofurfurylaniline

→

2-chloro-4-amino-N-tetrahydrofurfurylaniline monohydrochloride

Lösungsmittel

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThis mixture is heated to the reflux temperature
2. 2
   workup.ADDITIONWhen the addition
3. 3
   Filtrationthe latter is filtered
4. 4
   Sonstigethe filtrate is collected in 20 ml of ice-
5. 5
   Temperaturcooled hydrochloric acid
6. 6
   TemperaturAfter cooling
7. 7
   Sonstigethe expected hydrochloride precipitates in the form of crystals
8. 8
   FiltrationIt is filtered off
9. 9
   Waschenwashed with a small amount of ice-
10. 10
    Temperaturcooled absolute alcohol
11. 11
    Sonstigedried in vacuo

Vorschrift

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.

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