Reaktion #1463487

Reaktionsgleichung

7-chloro-1-methyl-5-phenyl-1H-1,4-benzodiazepine-2(3H)on

3-chloro-peroxybenzoic acid

→

7-chloro-1-methyl-5-phenyl-1H-1,4-benzodiazepine-2(3H)on-4-oxide

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITION27.303-1) are added
2. 2
   workup.STIRRINGStirring of the solution
3. 3
   WaschenThen the reaction mixture is washed first with 200 ml of 5% NH3 and subsequently with 200 μl of 0.1 n NaOH
4. 4
   SonstigeThe solvent is removed on an rotatione evaporator
5. 5
   workup.DISSOLUTIONthe remaining oily residue is dissolved in 25 ml of isopropanol
6. 6
   Temperaturunder heating to 40°-45° C
7. 7
   Sonstigeto crystallize
8. 8
   Temperaturunder slow cooling down to room temperature
9. 9
   Sonstige2 hours after the onset of crystallization
10. 10
    Waschenwashed with 50 ml of isopropanol and 50 ml of diisopropylether
11. 11
    TrocknenThe mixture is then dried over night over paraffin in an exsiccator

Vorschrift

5.70 g (20 mmol) of 7-chloro-1-methyl-5-phenyl-1H-1,4-benzodiazepine-2(3H)on (manufactured by Sigma, No. T 8275) are dissolved in 150 ml of dichloromethane and 13.8 g (40 mmol) of 3-chloro-peroxybenzoic acid (manufactured by Aldrich, No. 27.303-1) are added under stirring at 20° C. Stirring of the solution is continued for 1.5 h at 20° C. Then the reaction mixture is washed first with 200 ml of 5% NH3 and subsequently with 200 μl of 0.1 n NaOH. The solvent is removed on an rotatione evaporator and the remaining oily residue is dissolved in 25 ml of isopropanol under heating to 40°-45° C. Subsequently, the product is allowed to crystallize under slow cooling down to room temperature. 2 hours after the onset of crystallization, the solid product 2 is drawn off and washed with 50 ml of isopropanol and 50 ml of diisopropylether. The mixture is then dried over night over paraffin in an exsiccator.

Quelle