反应详情

温度

0 °C

{3-Phenyl-4-[(pyridin-2-ylmethyl)-amino]-thieno[2,3-b]pyridin-6-yl}-acetic acid ethyl ester (47 mg, 0.12 mmol) was dissolved in dry THF (10 ml) under nitrogen and cooled to 0° C. Diisobutyl Aluminium Hydride (0.466 ml of a 1 M solution in hexanes, 0.466 mmol) was added dropwise over 2 min and the mixture stirred at 0° C. for 1 h, then stirred at room temperature overnight. The reaction was cooled to 0° C. and water (5 ml) was added carefully, followed by 1 M Rochelle's salt (5 ml). The reaction was stirred at room temperature for 15 min, and then extracted with DCM (2×25 ml), the extracts combined, dried over magnesium sulphate, and concentrated. The residue was purified on silica, eluting (Ethyl Acetate/Petroleum ether), 50-100%) to give 2-{3-Phenyl-4-[(pyridin-2-ylmethyl)-amino]-thieno[2,3-b]pyridin-6-yl}-ethanol as a brown solid. Yield=25.3 mg (60.4%).

1. stirringstirred at room temperature overnight
2. temperatureThe reaction was cooled to 0° C.
3. stirringThe reaction was stirred at room temperature for 15 min
4. extractionextracted with DCM (2×25 ml)
5. dry with materialdried over magnesium sulphate
6. concentrationconcentrated
7. customThe residue was purified on silica
8. washeluting (Ethyl Acetate/Petroleum ether), 50-100%)