反应详情

A mixture of (6-benzyloxy-1H-indol-3-yl)-oxo-acetic acid methyl ester (1.45 g, 4.7 mmol) and Pd/C (10%, 0.9 g) in dioxane (38 mL) is degassed and filled with nitrogen for three times, then a solution of NaH2PO2 (6 g) in water (5 mL) is added dropwise at 100° C. The reaction mixture is heated overnight, filtered through celite and concentrated. The residue is taken into ethyl acetate, washed with water and brine, dried over sodium sulfate. Concentration and column chromatography on silica gel yields the title compound (600 mg).

1. customis degassed
2. additionfilled with nitrogen for three times
3. additiona solution of NaH2PO2 (6 g) in water (5 mL) is added dropwise at 100° C
4. temperatureThe reaction mixture is heated overnight
5. filtrationfiltered through celite
6. concentrationconcentrated
7. washwashed with water and brine
8. dry with materialdried over sodium sulfate
9. concentrationConcentration and column chromatography on silica gel