To separate the tertiary amines, the reaction mixture was treated with a mixture of acetic acid and acetic anhydride, excess of unreacted acetylating agent was removed, and the tertiary amines were isolated in the form of hydrochlorides. Dry hydrogen chloride was passed through the solution of the reaction mixture in ether or petroleum ether, or the reaction mixture was dissolved in a minimal amount
由于所得叔胺的沸点与初始仲烷基
甲胺的沸点相似,因此发现在反应结束时通过蒸馏分离这些化合物的常用方法是不合适的。为了分离叔胺,将反应混合物用
乙酸和
乙酸酐的混合物处理,除去过量的未反应的乙酰化剂,并以盐酸盐的形式分离叔胺。将干燥的
氯化氢通过反应混合物的
乙醚或石油醚溶液,或将反应混合物溶解在最少量的
盐酸中,用
乙醚或石油醚从
水溶液中萃取除去杂质。通过用碱
水溶液处理,然后蒸馏有机层,从盐酸盐中分离游离胺。新获得的叔胺的特征在 Tmble i 中给出,并且