(2-amino-5-bromophenyl)-phenylmethanol

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

実験手順: (2-Amino-5-bromo-phenyl)-phenyl-methanol (0.50 g, 1.798 mmol) is dissolved in anhydrous THF (25 mL). Triethylamine (0.55 g, 5.393 mmol) is added followed by triphosgene (0.16 g, 0.539 mmol). The mixture is stirred at room temperature overnight. Water (50 mL) is added and the reaction stirred for 15 minutes then extracted with ethylacetate (3×50 mL). The organic phases is washed with 1N HCl (2×50 mL) and a saturated solution of sodium hydrogencarbonate (50 mL). The organic phase is dried over sodium sulfate and concentrated in vacuo to provide the desired product as a white solid. the reaction stirred for 15 minutes then extracted with ethylacetate (3×50 mL) The organic phases is washed with 1N HCl (2×50 mL) The organic phase is dried over sodium sulfate concentrated in vacuo

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

実験手順: (2-Amino-5-bromo-phenyl)-phenyl-methanone (4.00 g, 14.49 mmol) is dissolved in methanol (50 mL). Sodium borohydride (0.55 g, 14.49 mmol) is added in small portions over 45 minutes. The reaction mixture is stirred at room temperature overnight. Water (10 mL) is added and the mixture stirred at room temperature for 15 minutes. The solvent is removed and the residue purified by column chromatography on silica gel using a petrol ether/ethylacetate gradient. This affords the desired compound as a white solid. the mixture stirred at room temperature for 15 minutes The solvent is removed the residue purified by column chromatography on silica gel using a petrol ether/ethylacetate gradient