37585-16-3 (2-氨基-4-氯苯基)甲醇

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合成路线 3（3. 合成：37585-16-3）

产率：69% 合成条件：Stage #1: With lithium aluminium tetrahydride In tetrahydrofuran at 0 - 20℃; for 2.17 h; Stage #2: With water; sodium sulfate In tetrahydrofuran at 0℃; 实验步骤：（2-氨基-4-氯苯基）甲醇。 在N 2下，在0℃下，将2-氨基-4-氯苯甲酸甲酯（1.5g，8.08mmol）的THF（15mL）溶液滴加到LAH（429mg，11.3mmol）的THF（10mL）悬浮液中。 10分钟 将所得混合物在室温下搅拌2小时，然后在0℃下用饱和Na 2 SO 4（50mL）淬灭反应，用Et 2 O（2.x.70mL）萃取。 将合并的有机溶液用盐水（30mL）洗涤，用MgSO 4干燥，并在旋转真空下浓缩，得到预期产物，为白色固体（874mg，69％收率）; 1H NMR（400MHz，MeOD）δppm4.50（s，2H），6.58（dd，J = 8.06,2.01Hz，1H），6.70（d，J = 2.01Hz，1H），7.01（d，J = 8.06） Hz，1H）; 质谱。 157.06（MH +），Calc。 C7H8ClNO 157.03。 参考文献：

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