3-氯-1H-吲哚-2-甲酸乙酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 3-chloro-1H-indole-2-carboxylate (19.28 mmol, 1.0 equiv.) was dissolved in THF-MeOH—H2O (2:1:1; 85 ml); LiOH.H2O (57.84 mmol, 3.0 equiv.) was added at 0° C. and the mixture was stirred for 12 h at 25° C. The solvent was reduced under reduced pressure, and the residue was taken up in water (50 ml), adjusted to pH 3 with 1 M HCl and extracted with ethyl acetate (2×100 ml). The combined organic phases were dried over Na2SO4 and concentrated under reduced pressure, and then the product was crystallized with hexane. Yield: 82% extracted with ethyl acetate (2×100 ml) The combined organic phases were dried over Na2SO4 concentrated under reduced pressure the product was crystallized with hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 1H-indole-2-carboxylate (26.45 mmol, 1.0 equiv.) was dissolved in CCl4 (26 ml); NCS (29.10 mmol, 1.1 equiv.) was added and the mixture was heated for 16 h at boiling temperature. The resulting solid was filtered out, and the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml), dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by column chromatography (10% ethyl acetate in hexane). Yield: 73% the mixture was heated for 16 h The resulting solid was filtered out the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml) dried over Na2SO4 concentrated under reduced pressure The crude product was purified by column chromatography (10% ethyl acetate in hexane)

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 1H-indole-2-carboxylate (26.45 mmol, 1.0 equiv.) was dissolved in CCl4 (26 ml); NCS (29.10 mmol, 1.1 equiv.) was added and the mixture was heated for 16 h at boiling temperature. The resulting solid was filtered out, and the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml), dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by column chromatography (10% ethyl acetate in hexane). Yield: 73% the mixture was heated for 16 h The resulting solid was filtered out the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml) dried over Na2SO4 concentrated under reduced pressure The crude product was purified by column chromatography (10% ethyl acetate in hexane)

反应条件: temp:25.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 3-chloro-1H-indole-2-carboxylate (19.28 mmol, 1.0 equiv.) was dissolved in THF-MeOH—H2O (2:1:1; 85 ml); LiOH.H2O (57.84 mmol, 3.0 equiv.) was added at 0° C. and the mixture was stirred for 12 h at 25° C. The solvent was reduced under reduced pressure, and the residue was taken up in water (50 ml), adjusted to pH 3 with 1 M HCl and extracted with ethyl acetate (2×100 ml). The combined organic phases were dried over Na2SO4 and concentrated under reduced pressure, and then the product was crystallized with hexane. Yield: 82% extracted with ethyl acetate (2×100 ml) The combined organic phases were dried over Na2SO4 concentrated under reduced pressure the product was crystallized with hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 1H-indole-2-carboxylate (26.45 mmol, 1.0 equiv.) was dissolved in CCl4 (26 ml); NCS (29.10 mmol, 1.1 equiv.) was added and the mixture was heated for 16 h at boiling temperature. The resulting solid was filtered out, and the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml), dried over Na2SO4 and concentrated under reduced pressure. The crude product was purified by column chromatography (10% ethyl acetate in hexane). Yield: 73% the mixture was heated for 16 h The resulting solid was filtered out the filtrate was washed with water (2×50 ml) and sat. NaCl solution (50 ml) dried over Na2SO4 concentrated under reduced pressure The crude product was purified by column chromatography (10% ethyl acetate in hexane)