Ammonium Hydroxide → HCID 23316356、化合物

反応式

[Cl:1][C:2]1[CH:16]=[CH:15][C:5]2[CH2:6][N:7]3[CH:14]=[CH:13][CH:12]=[C:8]3[C:9](=[O:11])[NH:10][C:4]=2[CH:3]=1.[Cl-:17].[Cl-].[Cl-].[Al+3].[OH-].[NH4+]>C(Cl)Cl>[Cl:17][C:13]1[CH:12]=[C:8]2[N:7]([CH:14]=1)[CH2:6][C:5]1[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][C:4]=1[NH:10][C:9]2=[O:11]

参加物

実験手順

To a solution of 2.33 g of 8-chloro-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepin-11-one in 50 mL of methylene chloride is added 5.33 g of aluminum trichloride. The reaction is stirred for 1 hour at room temperature and 0.77 mL (1.2 g) of methanesulfonyl chgloride is added. Stirring is then continued at room temperature overnight. The reaction mixture is basified with 10% ammonium hydroxide and the resulting solid collected by filtration. The solid is dissolved in methylene chloride, the solution is washed with water, dried over magnesium sulfate and evaporated to dryness to yield 2,8-dichloro-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]-benzodiazepin-11-one, which is used without further purification.