2-氨基-1,3,4-噻二唑是医药、染料中间体,用于染料及唑类药物合成,具有可燃性,燃烧产生有毒氮氧化物和硫氧化物烟雾,急性毒性数据为腹腔-大鼠LD50:200毫克/公斤,腹腔-小鼠LD50:6500毫克/公斤,储运需库房通风低温干燥,灭火剂可选用干粉、泡沫、砂土、二氧化碳、雾状水。
医药; 染料; 唑类药物合成
合成路线1
- 原料:氨基硫脲、甲酸、浓盐酸
- 步骤:称取5.00g氨基硫脲,置于50mL三颈烧瓶中,加入5.00mL甲酸,冰浴冷却搅拌成浆状物后,缓慢滴加6.00mL浓盐酸;滴毕转移至107℃油浴,搅拌反应4.5-5.0h,TLC监测至原料消失;冷却至室温,用浓氨水调pH至8-9,冰箱过夜析出晶体,过滤,冰水洗涤三次,蒸馏水重结晶得产物。
- 条件:反应温度107℃(油浴),冰浴冷却,反应时间4.5-5.0h,pH调节至8-9
- 收率:约90%(4.96g产物)
- 产物特性:白色晶体,熔点198-201℃,经IR、NMR、MS鉴定结构
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