摘要
2-甲基-2-(1-乙氧基乙氧基)-4-(苯基磺酰基)丁烷(简称C5缩醛砜),是一类重要的砜类化合物,可作为25-羟基维生素D3的C5片段中间体。在有机合成中,砜易于引入和脱去。以C5醇碘为原料,经羟基缩醛化和硫烷基化反应,制得C5缩醛砜。羟基缩醛化的催化剂为一水合对甲苯磺酸,反应适合在0~10℃进行,硫烷基化反应适合在70℃左右进行,往体系中加入碳酸钠可抑制缩醛保护基脱落,提高反应体系的水分可有效抑制氧烷基化副反应。
2-Methyl-2-(1-ethoxyethoxy)-4-(phenylsulfonyl)butane(abbreviated as C5 acetal sulfone) is an important class of sulfone compounds,which can be used as 25-hydroxyl Intermediate of the C5 fragment of vitamin D3.In organic synthesis,sulfone is easy to introduce and remove.C5 alcohol iodine is used as raw material,and C5 acetal sulfone is prepared through hydroxyl acetalization and sulfur alkylation reaction.The catalyst for the acetalization of the hydroxyl group is p-toluenesulfonic acid monohydrate,and the reaction is suitable to be carried out at 0-10°C.The sulfoalkylation reaction is suitable to be carried out at around 70°C.The addition of sodium carbonate to the system can inhibit the shedding of the acetal protective group,and increasing the water content of the reaction system can effectively inhibit the side reaction of oxyalkylation.
作者
方泽华
廖艳金
姚伟平
蒙美壮
Fang Zehua;Liao Yanjin;Yao Weiping;Meng Meizhuang(Guangzhou Juyuan Bio-chem Co.,Ltd.,Guangzhou 510700;Zhaoqing Juyuan Bio-chem Co.,Ltd.,Zhaoqing 526200,China)
出处
《广东化工》
CAS
2022年第14期8-10,共3页
Guangdong Chemical Industry
作者简介
方泽华(1987-),女,广东揭阳人,中级工程师,主要从事类胡萝卜素合成研究。
