반응 #2137698

반응 방정식

4,5-dihydro-5-thioxo-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

4,5-Dihydro-5-thioxo-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylene-3-one

sodium hydride

methyl iodide

→

desired product

5-(Methylthio)-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one

용매

tetrahydrofuran

반응 조건

후처리

1. 1
   온도to warm to room temperature
2. 2
   workup.STIRRINGis stirred for 3 hours
3. 3
   기타The mixture is quenched with water
4. 4
   추출extracted with chloroform and evaporation of the
5. 5
   추출extract in vacuo

실험 절차

To a solution of 100 mg of 4,5-dihydro-5-thioxo-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylen-3-one (Example 24) in 10 ml of dry tetrahydrofuran, cooled at 0° C., is added 13 mg of sodium hydride (60 percent dispersion in mineral oil). The reaction mixture is stirred at 0° C. for 15 minutes, then an excess of methyl iodide is added and the mixture is allowed to warm to room temperature and then is stirred for 3 hours. The mixture is quenched with water and extracted with chloroform and evaporation of the extract in vacuo gives 47 mg of the desired product mp 234-237° C. (with decomposition).

출처