吲哚酮的Mannich反应及其羟甲基化副产物的结构确证

Mannich reaction of 3-ethyl-1,5,6,7-tetrahydro- 2-methyl-4H-indol-4-one and the characterization of the hydroxymethylated by-product

在考察吗吲酮合成路线中Mannich反应的反应条件时 ,采用改变反应溶剂的方法 ,希望通过提高反应温度来提高收率。结果发现未进行Mannich反应 ,而进行羟甲基化副反应 ;产物经IR ,1H NMR ,13 C NMR ,MS确证为N 羟甲基 3 乙基 1,5 ,6 ,7 四氢 2 甲基 4H 吲哚 4 酮。因此 3 乙基 1,5 ,6 ,7 四氢 2 甲基 4H 吲哚 4 酮 (Ⅰ )与多聚甲醛、吗啉盐酸盐进行Mannich反应时 ,不能采用冰乙酸作溶剂。

To improve the yield of the Mannich reaction in the synthetic route of molindone by the reaction solvent was changed.When acetic acid was used as a solvent,the hydroxymethylation took place and the product was characterized to be N- hydroxymethyl-3-ethyl-1,5,6,7-tetrahydro-2-methyl-4H-indol-4-one.So do not use acetic acid as the reaction solvent in the Mannich reaction of 3-ethyl-1,5,6,7-tetrahydro-2-methyl-4H-indol-4-one.