反应详情

温度

35 °C

Method O—Step a To a vial with (R)-1-[4-Chloro-3-(5-methyl-1H-benzoimidazol-2-yl)-phenyl]-piperidine-3-carboxylic acid hydrochloride (obtained as described in general method 3,4, step e) (0.10 g, 0.25 mmol), HATU (0.10 g, 0.26 mmol), TEA (0.07 mL, 0.53 mmol) and 2-morpholin-4-yl-ethylamine (0.04 mL, 0.33 mmol), dichloromethane (2 mL) was added and the reaction mixture was heated at 35° C. overnight. Reaction was cooled to room temperature, saturated NaHCO3 solution (2 mL) was added with stirring, the organic layer recovered by filtration through phase separator, and the solvent removed under reduced pressure. The crude was purified by SCX and flash chromatography (eluent; gradient cyclohexane:ethylacetate from 100:0 to 3:1) to obtain 0.05 g of the title compound (42%).

1. customReaction
2. temperaturewas cooled to room temperature
3. filtrationthe organic layer recovered by filtration through phase separator
4. customthe solvent removed under reduced pressure
5. customThe crude was purified by SCX and flash chromatography (eluent; gradient cyclohexane:ethylacetate from 100:0 to 3:1)