乙基 2-(3-溴苯基)-2-羟基乙酸甲酯

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 3-Bromomandelic acid ethyl ester (0.5 g, 2.2 mmol) in THF (5 mL) at 0° C. was added sodium hydride (352 mg, 60% in mineral oil, 8.8 mmol) and the resulting mixture was stirred at 0° C. for 15 minutes. Methyl iodide (1.9 g, 13.2 mmol) was added and the resulting mixture was stirred at 0° C. for 10 minutes and warmed to room temperature for 15 minutes. Saturated sodium chloride (10 mL) was added and 1 N hydrochloric acid was added to adjust the pH to 4. The resulting mixture was extracted with ethyl acetate (5 mL×4) and the combined organic extracts were dried over sodium sulfate, filtered, and concentrated. The residue (0.43 g, 80%) was used in next step without further purification. MS: m/z 245 (M+H+). the resulting mixture was stirred at 0° C. for 10 minutes warmed to room temperature for 15 minutes The resulting mixture was extracted with ethyl acetate (5 mL×4) the combined organic extracts were dried over sodium sulfate filtered concentrated The residue (0.43 g, 80%) was used in next step without further purification

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 3-Bromomandelic acid ethyl ester (0.5 g, 2.2 mmol) in THF (5 mL) at 0° C. was added sodium hydride (352 mg, 60% in mineral oil, 8.8 mmol) and the resulting mixture was stirred at 0° C. for 15 minutes. Methyl iodide (1.9 g, 13.2 mmol) was added and the resulting mixture was stirred at 0° C. for 10 minutes and warmed to room temperature for 15 minutes. Saturated sodium chloride (10 mL) was added and 1 N hydrochloric acid was added to adjust the pH to 4. The resulting mixture was extracted with ethyl acetate (5 mL×4) and the combined organic extracts were dried over sodium sulfate, filtered, and concentrated. The residue (0.43 g, 80%) was used in next step without further purification. MS: m/z 245 (M+H+). the resulting mixture was stirred at 0° C. for 10 minutes warmed to room temperature for 15 minutes The resulting mixture was extracted with ethyl acetate (5 mL×4) the combined organic extracts were dried over sodium sulfate filtered concentrated The residue (0.43 g, 80%) was used in next step without further purification

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 3-Bromomandelic acid ethyl ester (0.5 g, 2.2 mmol) in THF (5 mL) at 0° C. was added sodium hydride (352 mg, 60% in mineral oil, 8.8 mmol) and the resulting mixture was stirred at 0° C. for 15 minutes. Methyl iodide (1.9 g, 13.2 mmol) was added and the resulting mixture was stirred at 0° C. for 10 minutes and warmed to room temperature for 15 minutes. Saturated sodium chloride (10 mL) was added and 1 N hydrochloric acid was added to adjust the pH to 4. The resulting mixture was extracted with ethyl acetate (5 mL×4) and the combined organic extracts were dried over sodium sulfate, filtered, and concentrated. The residue (0.43 g, 80%) was used in next step without further purification. MS: m/z 245 (M+H+). the resulting mixture was stirred at 0° C. for 10 minutes warmed to room temperature for 15 minutes The resulting mixture was extracted with ethyl acetate (5 mL×4) the combined organic extracts were dried over sodium sulfate filtered concentrated The residue (0.43 g, 80%) was used in next step without further purification