3-甲基-1-戊烯-4-炔-3-醇合成工艺的改进

Synthesis process improvement of 3-methyl-1-penten-4-yn-3-ol

以液氨和金属钙为原料通过氨基化制得氨基钙,经炔化得到乙炔钙,乙炔钙再与甲基乙烯酮反应制得乙炔醇钙盐,经水解、挥发氨、水蒸气蒸馏、萃取、回收溶剂、粗馏、精馏制得3-甲基-1-戊烯-4-炔-3-醇。考察金属试剂、催化剂硝酸高铁投入量、阻聚剂和萃取剂对合成及产物的影响。结果表明,选用金属钙作为金属试剂,催化剂硝酸高铁投入量为金属钙质量的0.8%,改性复合阻聚剂和CH2Cl2萃取剂较为合适。该工艺合成路线得到的3-甲基-1-戊烯-4-炔-3-醇纯度达98%以上,物质的量收率71.0%。

Amino calcium is prepared from liquid ammonia and metallic calcium through amination.Acetylene calcium is obtained through acetylation,and then reacts with methyl ketene to obtain acetylene calcium salt.3-methyl-1-penten-4-yne-3-ol is obtained through hydrolysis,volatilization of ammonia,steam distillation,extraction,solvent recovery,crude distillation,and distillation.The effects of metal reagent,catalyst,polymerization inhibitors and extractant on reaction and product were investigated.The results showed that it was more appropriate to choose metal calcium as metal reagent,modified composite polymerization inhibitor,CH 2 Cl 2 as extractant,and the optimal amount of catalyst for the metallization process was 0.8%of the mass of metallic calcium nitrate.The experiment showed that the GC purity of 3-methyl-1-penten-4-yne-3-ol synthesized by this process route was over 98%,and the molar yield was 71.04%.