摘要
用吲哚、二甲胺、甲醛、冰醋酸为原料合成3-二甲氨基甲基吲哚,最佳反应条件:配料比nC8HzN:n(CH)_3NH:nHCHO:nCH3COOH=1:1:1:2.5。在5℃时,二甲胺与冰醋酸混合均匀,再加入甲醛,吲哚,温度升至30℃,反应7小时。得到的液体冷至5℃,加入NaOH至pH=11,析出晶体。粗品水洗至pH=8,丙酮重结晶,干燥得产品。熔点:133.4℃,纯度:98％,以吲哚计算的收率84.5％。
The title compound was synthesized from dimethylamine, formaldehyde and glacial acetic acid. The optimum reaction conditions were: n(C8H7N): n[(CH3)2NH]: n(HCHO): n(CH3COOH)=1: 1: 1: 2.5. At5℃, dimethylamine and glacial acetic were mixed well, then added formaldehyde and indole. The temperature of the mixture rose to 30℃ during this period. The mixture was allowed to stand for 7 hrs, then cooled to 51℃. Sodium hydroxide was added to the mixture until pH=11,the solid crystallized out and treated with water to pH=8. recrystallized by acetone and drying overnight., mp 133.4℃, purity 98%. The yield was 84.5%(calcd. from indol).
出处
《染料工业》
2002年第6期28-29,共2页
Dyestuff Industry
