摘要
以对溴苯甲酸为起始原料,经酰化后生成酰氯,酰氯与N,O-二甲基羟胺盐酸盐反应生成酰胺,再与氯乙烯基镁反应生成α,β不饱和酮。同时,正戊醛与二正丙胺反应生成烯胺。α,β不饱和酮与烯胺经迈克尔加成反应生成分子内醛酮,分子内醛酮经关环反应、乙醇重结晶可得到色谱纯度99.5%以上的反-5-丙基-2-(4'-溴-苯基)-四氢吡喃。
The starting material of 4-bromobenzene carboxylic acid was acylated to generate acyl chloride.Then,acyl chloride reacted with N,O-dimethyl hydroxylamine hydrochloride to synthesize the amides,which then reacted with chlorovinylmagnesium to synthesize α,β unsaturated ketone.Meanwhile,allyl amine was synthesized from the reaction of pentanal with di-n-propylamine.By Michael addition reaction,α,β unsaturated ketone and allyl amine reacted to synthesize intramolecular aldehyde and ketone,which further reacted to synthesize trans-5-propyl-2-（4′-bromine-phenyl）-tetrahydropyran（3PyPBr） with a purity of more than 99.5% by closed loop reaction and recrystallization with ethanol.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2012年第10期1036-1040,共5页
Fine Chemicals
关键词
四氢吡喃型液晶
迈克尔加成
关环反应
精细化工中间体
tetrahydropyran-based liquid crystals
Michael addition
closed loop reaction
fine chemical intermediates
