反应详情

To 30 ml of tetrahydrofuran, 1.4 g of N-methylglycine ethyl ester was dissolved, and 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was gradually added thereto under stirring at room temperature. The mixture was stirred at room temperature for 1 hour, and the precipitated crystals were collected by filtration and recrystallized from acetone-ethyl ether, whereby 1.7 g (yield: 67%) of N-(1,3-dithiol-2-ylidene)-N-methyl-N-ethoxycarbonylmethylammonium perchlorate (Compound No. 1) was obtained as crystals having a melting point of from 104° to 105° C.

1. stirringThe mixture was stirred at room temperature for 1 hour
2. filtrationthe precipitated crystals were collected by filtration
3. customrecrystallized from acetone-ethyl ether