反应详情

A mixture of 3-ethoxy-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione (0.395 g, 0.0015 mol) and tert-amylamine (4 ml, 0.034 mol) in enough CH2 Cl2 to form a solution (a small amount of dry ethanol was required) was stirred at room temperature for two days. During this time, a precipitate forms. TLC (2:1 ethyl acetate:hexane) indicates a loss of starting material. The reaction is evaporated to a solid on a rotary evaporator. The solid is taken up in ethyl acetate and extracted well with 0.25N HCl. The organic layer is washed once with distilled water, dried (Na2SO4), and evaporated to a solid. The solid is collected and washed with diethyl ether to give 3-(tert-amylamino)-4-(2-hydroxy-4-cyanophenyl)amino-3-cyclobutene-1,2-dione, 0.253 g (0.00085 mol, 55%).

1. customThe reaction is evaporated to a solid on a rotary evaporator
2. extractionextracted well with 0.25N HCl
3. washThe organic layer is washed once with distilled water
4. dry with materialdried (Na2SO4)
5. customevaporated to a solid
6. customThe solid is collected
7. washwashed with diethyl ether