反应详情

8.9 gm (0.03 mol) of 1-(7,8-dimethoxy-1,3,4,5-tetrahydro-2H-3-benzazepin-2-on-3-yl)-3-chloro-propane were dissolved in 100 ml of methylene chloride; the solution was admixed at -60° C. with 2.1 ml of boron tribromide. After removing the cooling bath the reaction temperature rose to 20° C. and at this temperature the reaction mixture was stirred for 10 hours. The resulting resinous precipitate was made to crystallize by addition of 100 ml of water and subsequent stirring for one hour. The crystalline precipitate was suction-filtered off and washed with water and methylene chloride. For purification the crystalline product was stirred with acetone and suction-filtered off.

1. customAfter removing the cooling bath the reaction temperature
2. customrose to 20° C. and at this temperature
3. customto crystallize by addition of 100 ml of water
4. stirringsubsequent stirring for one hour
5. filtrationThe crystalline precipitate was suction-filtered off
6. washwashed with water and methylene chloride
7. customFor purification the crystalline product
8. stirringwas stirred with acetone
9. filtrationsuction-filtered off