反应详情

温度

0 °C

(S)-Azepane-1-carboxylic acid (1-{4-[(4-amino-phenyl)-(3-methyl-butyl)-amino]-piperidine-1-carbonyl}-3-methyl-butyl)-amide (Example 35, 0.25 g, 0.50 mmol) was dissolved in CH2Cl2 (4 mL), treated with isovaleraldehyde (63 μL, 0.50 mmol), and stirred for 30 minutes. The reaction was cooled to 0° C., treated with NaBH(OAc)3 (0.16 g, 0.75 mmol), and allowed to warm to room temperature and stir overnight. The reaction was diluted with EtOAc (100 mL), washed with saturated bicarbonate solution and brine, dried over Na2SO4, and concentrated. The residue was chromatographed on silica gel eluting with 4% to 5% MeOH/CH2Cl2 to give the desired product.

1. temperatureto warm to room temperature
2. stirringstir overnight
3. washwashed with saturated bicarbonate solution and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customThe residue was chromatographed on silica gel eluting with 4% to 5% MeOH/CH2Cl2