反应详情

A solution of 1.2 g of triethylamine in 10 ml of dry ether was added dropwise to a mixture of 2.4 g of 2,6-di-t-butyl-4-nitrosophenol and 2.7 g of N-[[[N-[[N-fluorocarbonyl-N-methylaminothio]]-N-methylaminocarbonyloxy]]]ethanimidothioic acid methyl ester suspended in 40 ml of dry ether at a temperature below 25°. The mixture was stirred at room temperature for 50 minutes. Then, water and hexane were added to the mixture. The product was collected by filtration, washed with water, hexane, and air-dried to give 4.1 g of N-[[[N-[[3,5-bis-(1,1-dimethylethyl)-4-oxo-2,5-cyclohexadien-1-yli-deneaminooxycarbonyl]-N-methylaminothio]]-N-methylaminocarbonyloxy]]ethanimidothioic acid methyl ester, m.p. 160°-161.6°.

1. filtrationThe product was collected by filtration
2. washwashed with water, hexane
3. customair-dried