ethyl 6-fluoro-1-benzofuran-3-carboxylate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1M LiAlH4-solution in THF (75.9 ml, 75.9 mmol) is diluted with 100 ml of THF and cooled to 0° C. 110 (7.9 g, 37.9 mmol) is dissolved in 100 ml of THF and added dropwise within 30 min. After completed addition the mixture is allowed to stir at rt for 2 h. Then the reaction mixture is cooled to −15° C. and 10 ml of a 1M NaOH solution is added very slowly. The mixture is filtrated over celite and evaporation under reduced pressure gave 5.3 g of a yellow oil. added dropwise within 30 min addition the mixture Then the reaction mixture is cooled to −15° C. The mixture is filtrated over celite and evaporation under reduced pressure

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1M LiAlH4-solution in THF (75.9 ml, 75.9 mmol) is diluted with 100 ml of THF and cooled to 0° C. 110 (7.9 g, 37.9 mmol) is dissolved in 100 ml of THF and added dropwise within 30 min. After completed addition the mixture is allowed to stir at rt for 2 h. Then the reaction mixture is cooled to −15° C. and 10 ml of a 1M NaOH solution is added very slowly. The mixture is filtrated over celite and evaporation under reduced pressure gave 5.3 g of a yellow oil. added dropwise within 30 min addition the mixture Then the reaction mixture is cooled to −15° C. The mixture is filtrated over celite and evaporation under reduced pressure

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1M LiAlH4-solution in THF (75.9 ml, 75.9 mmol) is diluted with 100 ml of THF and cooled to 0° C. 110 (7.9 g, 37.9 mmol) is dissolved in 100 ml of THF and added dropwise within 30 min. After completed addition the mixture is allowed to stir at rt for 2 h. Then the reaction mixture is cooled to −15° C. and 10 ml of a 1M NaOH solution is added very slowly. The mixture is filtrated over celite and evaporation under reduced pressure gave 5.3 g of a yellow oil. added dropwise within 30 min addition the mixture Then the reaction mixture is cooled to −15° C. The mixture is filtrated over celite and evaporation under reduced pressure

反応条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 109 (40 g, 142.7 mmol) is dissolved in 300 ml of a DMSO and after addition of sodium chloride (16.7 g, 285.4 mmol) and water (5.1 ml) the mixture is stirred for 4 h at 160° C. (temperature of reaction mixture). Then the mixture is allowed to cool down and evaporated at high vacuum. The residue is dissolved in ethyl acetate, washed with water and brine and dried over sodium sulfate. Evaporation gave 14.8 g of an red oil, which is further purified by filtration over silica gel (ethyl acetate/hexanes 2:8). (temperature of reaction mixture) to cool down evaporated at high vacuum The residue is dissolved in ethyl acetate washed with water and brine dried over sodium sulfate Evaporation

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1M LiAlH4-solution in THF (75.9 ml, 75.9 mmol) is diluted with 100 ml of THF and cooled to 0° C. 110 (7.9 g, 37.9 mmol) is dissolved in 100 ml of THF and added dropwise within 30 min. After completed addition the mixture is allowed to stir at rt for 2 h. Then the reaction mixture is cooled to −15° C. and 10 ml of a 1M NaOH solution is added very slowly. The mixture is filtrated over celite and evaporation under reduced pressure gave 5.3 g of a yellow oil. added dropwise within 30 min addition the mixture Then the reaction mixture is cooled to −15° C. The mixture is filtrated over celite and evaporation under reduced pressure

反応条件: temp:160.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 109 (40 g, 142.7 mmol) is dissolved in 300 ml of a DMSO and after addition of sodium chloride (16.7 g, 285.4 mmol) and water (5.1 ml) the mixture is stirred for 4 h at 160° C. (temperature of reaction mixture). Then the mixture is allowed to cool down and evaporated at high vacuum. The residue is dissolved in ethyl acetate, washed with water and brine and dried over sodium sulfate. Evaporation gave 14.8 g of an red oil, which is further purified by filtration over silica gel (ethyl acetate/hexanes 2:8). (temperature of reaction mixture) to cool down evaporated at high vacuum The residue is dissolved in ethyl acetate washed with water and brine dried over sodium sulfate Evaporation