反应详情

To a solution of Cis-2-Chloro-N-(4-formyl-cyclohexyl)-5-trifluoromethyl-benzamide (100 mg, 0.300 mmol) in DCM (3 mL) is added 3-(4-fluorophenyl)-1H-pyrazol-5-amine (58.4 mg, 0.330 mmol) to give a pale orange solution. This is stirred for 10 mins at room temperature before sodium triacetoxyborohydride (102 mg, 0.479 mmol) is added. The reaction mixture is stirred at room temperature for 1 hour. The reaction mixture is quenched by the addition of saturated sodium bicarbonate. The DCM layer is separated and further washed with water. The aqueous extracts are combined and re-extracted with DCM. The combined organic extracts are then dried over MgSO4, filtered and concentrated under vacuum. Purification by chromatography on a pre-packed 12 g silica gel column using 0-100% EtOAc in isohexane (gradient elution) gave the desired product as a colourless solid. [MH+495.29].

1. customto give a pale orange solution
2. additionis added
3. customThe reaction mixture is quenched by the addition of saturated sodium bicarbonate
4. customThe DCM layer is separated
5. washfurther washed with water
6. extractionre-extracted with DCM
7. dry with materialThe combined organic extracts are then dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated under vacuum
10. customPurification by chromatography on a pre-packed 12 g silica gel column