반응 #1463487

반응 방정식

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

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.ADDITION27.303-1) are added
2. 2
   workup.STIRRINGStirring of the solution
3. 3
   세척Then the reaction mixture is washed first with 200 ml of 5% NH3 and subsequently with 200 μl of 0.1 n NaOH
4. 4
   기타The solvent is removed on an rotatione evaporator
5. 5
   workup.DISSOLUTIONthe remaining oily residue is dissolved in 25 ml of isopropanol
6. 6
   온도under heating to 40°-45° C
7. 7
   기타to crystallize
8. 8
   온도under slow cooling down to room temperature
9. 9
   기타2 hours after the onset of crystallization
10. 10
    세척washed with 50 ml of isopropanol and 50 ml of diisopropylether
11. 11
    건조The mixture is then dried over night over paraffin in an exsiccator

실험 절차

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.

출처