반응 #63916

반응 방정식

methyl iodide

[3-(3-methyl-1,2,4-triazolo[4,3-b]-pyridazin-6-yl)phenyl]carbamic acid, ethyl ester

sodium hydride

dimethylformamide

→

off-white powder

Methyl[3-(3-methyl-1,2,4-triazolo[4,3-b]pyridazin-6-yl)phenyl]carbamic acid, ethyl ester

용매

water

반응 조건

후처리

1. 1
   workup.STIRRINGThis mixture was stirred overnight
2. 2
   추출extracted with 150 ml portions of dichloromethane
3. 3
   기타dried
4. 4
   농축concentrated in vacuo
5. 5
   기타The residue was chromatographed on 300 g of silica gel with dichloromethane-methanol (97:3)
6. 6
   workup.ADDITIONThe fractions containing product
7. 7
   기타the solvent evaporated in vacuo
8. 8
   기타the solid recrystalized from dichloromethane-hexane

실험 절차

A mixture of 1.5 g of [3-(3-methyl-1,2,4-triazolo[4,3-b]-pyridazin-6-yl)phenyl]carbamic acid, ethyl ester, 0.29 g of sodium hydride (50% in oil) and 150 ml of dimethylformamide was stirred under argon for 1 hour and then 0.38 ml methyl iodide was added. This mixture was stirred overnight then poured onto 500 ml of water and extracted with 150 ml portions of dichloromethane. The extracts were combined, dried and concentrated in vacuo. The residue was chromatographed on 300 g of silica gel with dichloromethane-methanol (97:3). The fractions containing product were combined, the solvent evaporated in vacuo and the solid recrystalized from dichloromethane-hexane, to give 1.25 g of an off-white powder, mp 146°-149° C.

출처