反应详情

温度

110 °C

A mixture of 1000 mg of rac-toluene-4-sulfonic acid (1R*,8R*,9R*)-2-(9-hydroxy-tricyclo[6.2.2.02,7]dodeca-2,4,6-trien-9-yl)ethyl ester and 508 mg of [3-(1H-benzoimidazol-2-yl)-propyl]-methyl-amine in 2 mL of DIPEA was heated to 110° C. for 30 min. The reaction mixture was cooled to rt, quenched with MeOH-water and extracted with EtOAc. The organic phase was separated, dried over Na2SO4 and concentrated in vacuo to obtain 1.0 g as beige solid. A part of the crude product was purified by CC with EtOAc/MeOH (2:1) to obtain the desired compound as beige foam.

1. temperatureThe reaction mixture was cooled to rt
2. customquenched with MeOH-water
3. extractionextracted with EtOAc
4. customThe organic phase was separated
5. dry with materialdried over Na2SO4
6. concentrationconcentrated in vacuo
7. customto obtain 1.0 g as beige solid
8. customA part of the crude product was purified by CC with EtOAc/MeOH (2:1)