反应详情

温度

35 °C

A mixture of 1 g (0.0046 mol) of 6-hydroxy-quinoline-2-carboxylic acid ethyl ester, 2.4 g (0.0092 mol) of triphenylphospine (Fluka), 2.4 g (0.0092 mol) of 1-isopropyl-piperidin-4-ol and 1.6 ml (0.0092 mol) of di-tert.-butyl azadicarboxylate 40% in toluene in 100 ml THF was stirred for a prolonged period of time at 35° C. The mixture was filtered through a pad of silica and washed with 30 ml THF. The mixture was evaporated to dryness and purified on silica eluting with a gradient of DCM/MeOH 98/2. The product fractions were evaporated and the residue was triturated with diethyl ether to yield after drying under vacuum 1.3 mg (83%) of the title compound as white solid. MS (m/e): 343.3 (M+H)+.

1. filtrationThe mixture was filtered through a pad of silica
2. washwashed with 30 ml THF
3. customThe mixture was evaporated to dryness
4. custompurified on silica eluting with a gradient of DCM/MeOH 98/2
5. customThe product fractions were evaporated
6. customthe residue was triturated with diethyl ether
7. customto yield
8. dry with materialafter drying under vacuum 1.3 mg (83%) of the title compound as white solid