393-52-2 邻氟苯甲酰氯

危险品运输编号UN 3265 8/PG 2，危险等级8，包装类别II，海关编码29163900，存储类别8A（可燃，腐蚀性物质），危险性类别皮肤腐蚀类别1B，危险标志GHS05（腐蚀性）、GHS07（刺激性），危险性描述H314（造成严重皮肤灼伤和腐蚀）、H335（可能引起呼吸道刺激），防范说明P261（避免吸入粉尘/烟雾）、P280（戴防护手套/护目镜/面罩）、P305+P351+P338（眼睛接触后立即冲洗）、P310（立即就医）。非危险化学品描述存在矛盾。

邻氟苯甲酰氯主要用作医药、农药、染料中间体，用于化学合成反应。

医药; 农药; 染料

合成路线 1（中间体a：2-氟苯甲酰氯）

• 步骤: 向100mL甲苯中加入0.714mol（100g）2-氟苯甲酸，加热至50℃后缓慢加入5.7mol（414mL）氯化亚砜，反应混合物在回流条件下反应7小时。反应完成后蒸发去除过量氯化亚砜，得到79g 2-氟苯甲酰氯。
• 条件: 50℃加热，回流7小时；溶剂为甲苯；反应物摩尔比：2-氟苯甲酸:氯化亚砜≈1:8（0.714mol:5.7mol）。
• 产率: 70%。
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合成路线 2（中间体a：2-氟苯甲酰氯）

• 步骤: 取步骤（1）中得到的2.97 mol邻氯三氯苯搅拌至125130℃，保持微负压（00.5 cm水柱），缓慢滴加0.5％氯化锌水溶液，3小时滴完，保持反应温度125-130℃，保温1小时。GC跟踪反应，直至邻氟-三氯苯完全转化。采用真空蒸馏法纯化，收集100~105℃馏分，得到416.6g邻氟苯甲酰氯。
• 条件: 125-130℃反应，微负压（0~0.5 cm水柱），滴加0.5％氯化锌水溶液3小时，保温1小时；溶剂为邻氯三氯苯（原料）。
• 产率: 98%（纯度99.5%）。
• 参考文献: [1] Patent: CN106008197, 2016, A. Location in patent: Paragraph 00119; 0020。