化学合成。
化学合成
合成路线 1(1. 合成:304873-65-2)
产率:84%
合成条件:With sodium hydrogencarbonate In dichloromethane; water at 0℃; for 1 h;
实验步骤:向步骤2的产物(19.15g,85.5 [MMOL]]的[CH 2 Cl 2](640ml)溶液中加入饱和的[NAHC03]水溶液(8.62g,103 [MMOL]]和NaBr(444mg) ,4.3 [MMOL]。]将反应混合物冷却至0 [℃],并引入TEMPO(140mg,0.90 [MMOL]]。 在剧烈搅拌下,在40分钟内分批加入市售漂白溶液(122 [ML,] 0.7 [M,] 85.4 [MMOL]](5.21%NaOCl)。 在0 [℃]下再过20分钟后,将反应混合物用饱和Na 2 S 2 O 3水溶液淬灭,并使其温热至23 [℃]。用水稀释并用CH 2 Cl 2萃取,然后浓缩并进行快速色谱(洗脱液:30%) [己烷-CH 2 Cl 2]至0-2%[ACETONE-CH 2 Cl 2]],得到15.97g(71.9 [MMOL]; 84%收率)醛,为灰白色固体。
参考文献:
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