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

HRID 2073191

Reaktionsgleichung

[S:1]=[C:2]1[N:12]2[C:13]3[N:8]([C:9]([C:14]4[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:23])([F:22])[F:21])[CH:15]=4)=[CH:10][CH2:11]2)[N:7]=[CH:6][C:5]=3[C:4](=[O:24])[NH:3]1.[H-].[Na+].[CH3:27]I>O1CCCC1>[CH3:27][S:1][C:2]1[N:12]2[C:13]3[N:8]([C:9]([C:14]4[CH:19]=[CH:18][CH:17]=[C:16]([C:20]([F:21])([F:22])[F:23])[CH:15]=4)=[CH:10][CH2:11]2)[N:7]=[CH:6][C:5]=3[C:4](=[O:24])[N:3]=1

Komponenten

Reaktionsbedingungen

Temperatur: 0 °C

Versuchsvorschrift

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).

Aufarbeitung

temperatureto warm to room temperature
stirringthen was stirred for 3 hours
customThe mixture was quenched with water
extractionextracted with chloroform
customEvaporation of the
extractionextract in vacuo

Quellen und Nachweise

ORD-Eintrag: ord-6573babafd70489ab5943058e8f585e0
Quelldatensatz: uspto-grants-1990_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US04916137

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