반응 #345720

반응 방정식

7-chloro-5-phenyl-1H-1,5-benzodiazepin-4-one-2-thione

sodium hydroxide

methyl iodide

→

2-(Methylthio)-7-chloro-5-phenyl-3H-1,5-benzodiazepin-4-one

용매

methanol

methanol

반응 조건

후처리

1. 1
   기타the reaction is then evaporated
2. 2
   여과The suspension is filtered through a short Florisil column
3. 3
   세척the column is washed with ethyl acetate
4. 4
   기타the combined filtrates are evaporated
5. 5
   기타The residue is triturated with a minimum amount of absolute ethanol
6. 6
   여과the title compound is filtered off
7. 7
   기타dried

실험 절차

To 3.03 g of 7-chloro-5-phenyl-1H-1,5-benzodiazepin-4-one-2-thione in a solution of 0.40 g of sodium hydroxide and 15 ml of methanol is added, with stirring a solution of 1.4 g of methyl iodide in 10 ml of methanol. Stirring is continued for 1 hour, the reaction is then evaporated and suspended in methylene chloride (30 ml). The suspension is filtered through a short Florisil column; the column is washed with ethyl acetate and the combined filtrates are evaporated. The residue is triturated with a minimum amount of absolute ethanol and the title compound is filtered off and dried.

출처