反应详情

温度

80 °C

2-Cyano-N-cyclopropyl-N-(2,3-dichlorobenzyl)-3-[4-(3-hydroxypropyl)phenyl]-2-methylpropanamide from the previous step (1 eq.) and 2-chloro-3,6-difluorphenol (4 eq.) were taken up in freshly deoxygenated toluene (0.05 M). To this solution was then added 1,1′-(azodicarbonyl)-dipiperidine (4 eq.) and finally tributylphosphine (4 eq.). The resulting yellow solution was heated at 80° C. for 3 h. The reaction mixture was cooled to RT, diluted with ether, and washed with 1 N aq. NaOH. The aqueous wash was back extracted with ether and the combined organic extracts were dried over MgSO4. Filtration and concentration of the filtrate in vacuo afforded a yellow semi-solid. Purification of the crude product thus obtained by way of flash chromatography (SiO2, Hex→3:2 (v/v) Hex:EtOAc) afforded the title compound as a colorless oil.

1. temperatureThe reaction mixture was cooled to RT
2. washwashed with 1 N aq. NaOH
3. washThe aqueous wash
4. extractionwas back extracted with ether
5. dry with materialthe combined organic extracts were dried over MgSO4
6. filtrationFiltration and concentration of the filtrate in vacuo
7. customafforded a yellow semi-solid
8. customPurification of the crude product
9. customthus obtained by way of flash chromatography (SiO2, Hex→3:2 (v/v) Hex:EtOAc)