반응 #2160373

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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-tetraazaacenaphthylen-3-one

sodium hydride

methyl iodide

→

product

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

용매

tetrahydrofuran

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후처리

1. 1
   온도to warm to room temperature
2. 2
   workup.STIRRINGthen was stirred for 3 hours
3. 3
   기타The mixture was quenched with water
4. 4
   추출extracted with chloroform
5. 5
   기타Evaporation of the
6. 6
   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 8) in 10 ml of dry tetrahydrofuran, cooled at 0° C., was added 13 mg of sodium hydride (60% dispersion in mineral oil). The reaction mixture was stirred at 0° C. for 15 minutes, then an excess of methyl iodide was added. The mixture was allowed to warm to room temperature then was stirred for 3 hours. The mixture was quenched with water and extracted with chloroform. Evaporation of the extract in vacuo gave 47 mg of the product of the example as a yellow solid, m.p. 234°-237° C. (dec).

출처