反应详情

温度

0 °C

To a solution of the (R)-2-hydroxy-3-(7-methyl-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-5-yl)propanoic acid (610 mg, 1.74 mmol), diisopropylethylamine (0.61 mL, 3.48 mmol), and 4-piperidinopiperidine (585.76 mg, 2.0 equiv) in dimethylformamide (20 mL) and dichloromethane (20 mL) at 0° C. was added PyBOP® (951 mg, 1.83 mmol). The reaction was stirred at 0° C. for 2 h. The reaction was concentrated, diluted with ethyl acetate, washed with water, then brine, dried over magnesium sulfate, and concentrated. The product was purified by column chromatography (4:96:1 methanol/dichloromethane/triethylamine) to give 795 mg (91%). Mass spec.: 501.40 (MH)+.

1. concentrationThe reaction was concentrated
2. additiondiluted with ethyl acetate
3. washwashed with water
4. dry with materialbrine, dried over magnesium sulfate
5. concentrationconcentrated
6. customThe product was purified by column chromatography (4:96:1 methanol/dichloromethane/triethylamine)
7. customto give 795 mg (91%)