反应详情

To a CH2Cl2 solution (0.1 M) of 3-[3-(methyloxy)propyl]-1-naphthalenecarboxylic acid (1 eq.) from the previous step was added at 0° C. oxalyl chloride (1.2 eq.) followed by a few drops of DMF. The resulting solution was stirred at RT for 2 h before the volatiles were removed in vacuo. The resulting residue was taken up in dichloromethane (0.1 M), cooled to 0° C. and added sequentially Hunig's base (1.2 eq.) an cyclopropylamine (1.1 eq.) dropwise. The resulting suspension was stirred at RT for 18 h. The reaction was quenched with 1 N aq. HCl and extracted with ether. The combined organic extracts were washed further with 1 N aq. NaOH, water and brine, dried over Na2SO4 and filtered. Concentration of the filtrate in vacuo afforded the title compound as a white solid.

1. customwere removed in vacuo
2. temperaturecooled to 0° C.
3. stirringThe resulting suspension was stirred at RT for 18 h
4. customThe reaction was quenched with 1 N aq. HCl
5. extractionextracted with ether
6. washThe combined organic extracts were washed further with 1 N aq. NaOH, water and brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered