反应详情

From N-benzyl-N-tert-butylcarbonyl-N-[(2S)-5-(1,3,5-trimethyl-1H-pyrazol-4-yl)-1,2,3,4-tetrahydronaphthalen-2-yl]amine: TFA (0.330 mL, 4.275 mmol) was added to a 0° C. cooled solution of starting material (0.381 g, 0.855 mmol) in CH2Cl2 (15 mL). The reaction was allowed to reach room temperature, and stirred at this temperature for 7 h. It was poured into H2O (20 mL), extracted with CH2Cl2 (1×25 mL) and washed with NaOH aqueous solution (10%, 2×20 mL). The organic layer was dried over anhydrous Na2SO4, filtered and concentrated. The crude residue was flash chromatographed on silica gel (0-5-10% MeOH/CH2Cl2) to give 0.215 g of the title product (Rf=0.2 (10% MeOH/CH2Cl2), yellow oil, 73% yield).

1. customto reach room temperature
2. extractionextracted with CH2Cl2 (1×25 mL)
3. washwashed with NaOH aqueous solution (10%, 2×20 mL)
4. dry with materialThe organic layer was dried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customchromatographed on silica gel (0-5-10% MeOH/CH2Cl2)