Reaktion #95428

Reaktionsgleichung

4-chloro-3-nitro-benzophenone

methylamine

sulpholane

→

4-methylamino-3-nitro-benzophenone

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe reaction solution is evaporated to dryness
2. 2
   Filtrationthe precipitate is filtered off
3. 3
   Waschenwashed with water
4. 4
   workup.DISSOLUTIONdissolved in methylene chloride
5. 5
   TrocknenAfter drying over sodium sulphate
6. 6
   Sonstigeevaporating

Vorschrift

11 g of 4-chloro-3-nitro-benzophenone, 20 g of methylamine, 153.4 g of methanol and 27.5 g of sulpholane are warmed to 125° for 15 hours in a closed vessel. The reaction solution is evaporated to dryness, the residue is boiled thoroughly with 400 ml of 2 N hydrochloric acid for 20 minutes and the precipitate is filtered off, washed with water and dissolved in methylene chloride. After drying over sodium sulphate and evaporating, 4-methylamino-3-nitro-benzophenone with a melting point of 198°-201° is obtained.

Quelle