反应详情

The amine (Reference Example 7, 0.048 g, 0.11 mM) was refluxed in ethyl formate (3 ml). After 2 hours, chloroform (1 ml) and dichloromethane (1 ml) was added to solublise the precipitate. After 70 hours the solution was evaporated and the residue dissolved in acetonitrile/EtOAc (1:1) and the precipitate removed by filtration. The mother liquor was purified by Isolute chromatography (using as eluant a mixture increasing in polarity from 50% to 70% MeCN in EtOAc) to give after trituration with diethyl ether the title product (0.010 g, 20%).

1. customAfter 70 hours the solution was evaporated
2. dissolutionthe residue dissolved in acetonitrile/EtOAc (1:1)
3. customthe precipitate removed by filtration
4. customThe mother liquor was purified by Isolute chromatography (
5. temperatureincreasing in polarity from 50% to 70% MeCN in EtOAc)