反应详情

温度

100 °C

Combine 5-amino-3-(4-tert-butyl-phenyl)-4-cyano-thiophene-2-carboxylic acid methyl ester (0.29 mmol) in acetonitrile and add diiodomethane (1.02 mmol) and iso-amyl nitrite (0.73 mmol) and heat to 100° C. After 15 minutes, cool the reaction slowly to room temperature and stir an additional 1 hour. Concentrate the reaction to a dark oil which is purified by radial chromatography on a 2000 micron silica plate eluting with 50/50 methylene chloride/hexane and then 100% methylene chloride. Concentrate desired fractions were to give the title compound. 1H NMR (400 MHz, CDCl3) δ 7.41 (m, 4H), 3.78 (s, 3H), 1.37 (s, 9H).

1. temperaturecool
2. customthe reaction slowly to room temperature
3. concentrationConcentrate
4. customthe reaction to a dark oil which
5. customis purified by radial chromatography on a 2000 micron silica plate
6. washeluting with 50/50 methylene chloride/hexane
7. concentrationConcentrate desired fractions