反应详情

To 10 ml of tetrahydrofuran, 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was suspended, and 0.75 ml of dibutylamine was dropwise added over a period of 5 minutes. The mixture was stirred at room temperature for 30 minutes, and the solvent was distilled off under reduced pressure. The residue was dissolved in a mixture of acetone-ethyl ether, and cooled to -70° C. in a cooling medium, whereupon crystals precipitated. The crystals were collected by decantation under cooled condition, and purified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50), whereby 0.20 g (yield: 75%) of N-(1,3-dithiol-2-ylidene)-N,N-di(n-butyl)ammonium perchlorate was obtained as oily substance. (Compound No. 23)

1. distillationthe solvent was distilled off under reduced pressure
2. dissolutionThe residue was dissolved in a mixture of acetone-ethyl ether
3. temperaturecooled to -70° C. in a cooling medium, whereupon crystals
4. customprecipitated
5. customThe crystals were collected by decantation
6. temperatureunder cooled condition
7. custompurified by liquid chromatography (column: Senshu pack, Senshu ODS-5301, mobile phase: methanol/water=50/50)