广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2014年
16期
80-82
,共3页
阿利克伦中间体%合成%柱层析
阿利剋倫中間體%閤成%柱層析
아리극륜중간체%합성%주층석
aliskiren intermediates%synthesis%column chromatography
以异香草醛为原料通过醚化、还原、甲基醚化、溴代、亲电取代、氧化、还原等多步法合成阿里克伦中间体1-氯-2R-[4-甲氧基-3-(3-甲氧基丙氧基)苄基]-3-甲基丁烷粗品,粗品采用柱层析法分离,分离得到阿利克仑中间体纯度为98.3%,回收率达90.4%。通过实验室合成及建立较简单的分离工艺,为工业生产、提纯阿利克仑中间体提供了可靠的实验依据。
以異香草醛為原料通過醚化、還原、甲基醚化、溴代、親電取代、氧化、還原等多步法閤成阿裏剋倫中間體1-氯-2R-[4-甲氧基-3-(3-甲氧基丙氧基)芐基]-3-甲基丁烷粗品,粗品採用柱層析法分離,分離得到阿利剋崙中間體純度為98.3%,迴收率達90.4%。通過實驗室閤成及建立較簡單的分離工藝,為工業生產、提純阿利剋崙中間體提供瞭可靠的實驗依據。
이이향초철위원료통과미화、환원、갑기미화、추대、친전취대、양화、환원등다보법합성아리극륜중간체1-록-2R-[4-갑양기-3-(3-갑양기병양기)변기]-3-갑기정완조품,조품채용주층석법분리,분리득도아리극륜중간체순도위98.3%,회수솔체90.4%。통과실험실합성급건립교간단적분리공예,위공업생산、제순아리극륜중간체제공료가고적실험의거。
Using isovanillin as raw material , through the reduction of etherification , methyl etherification , bromination, oxidation, reduction, dear electricity multi step synthesis of aliskiren intermediate 1-chloro-2R-[4-methoxy-3 -( 3 -methoxy propoxy ) benxyl ] -3 -methyl butane crude , crude product by column chromatography separation, separation of aliskiren intermediate purity was 98.3% and the recovery rate was 90.4%.Through the establishment of separation process synthesis and relatively simple laboratory , the reliable experimental basis was proposed for industrial production and purification of aliskiren intermediates.