广州化工
廣州化工
엄주화공
GUANGZHOU CHEMICAL INDUSTRY AND TECHNOLOGY
2015年
16期
116-117,167
,共3页
异戊二烯%中间体%4-乙酰氧基-2-甲基-2-丁烯-1-醛%合成
異戊二烯%中間體%4-乙酰氧基-2-甲基-2-丁烯-1-醛%閤成
이무이희%중간체%4-을선양기-2-갑기-2-정희-1-철%합성
isoprene%intermediate%4-acetoxy-2-methyl-2-butenal%synthesis
以异戊二烯为原料,与三氯异氰尿酸发生氯醇化反应,生成1,2加成和1,4加成产物混合物,加成产物混合物在浓硫酸为催化剂的条件下与乙酸酐发生酯化反应,酯化结束后直接升温进行转位反应生成1-乙酰氧基-4-氯-3-甲基-2-丁烯。之后在复合催化剂磷酸氢二钾、磷酸二氢钾和二甲基亚砜的条件下,用TEMPO氧化为目标产物4-乙酰氧基-2-甲基-2-丁烯-1-醛。
以異戊二烯為原料,與三氯異氰尿痠髮生氯醇化反應,生成1,2加成和1,4加成產物混閤物,加成產物混閤物在濃硫痠為催化劑的條件下與乙痠酐髮生酯化反應,酯化結束後直接升溫進行轉位反應生成1-乙酰氧基-4-氯-3-甲基-2-丁烯。之後在複閤催化劑燐痠氫二鉀、燐痠二氫鉀和二甲基亞砜的條件下,用TEMPO氧化為目標產物4-乙酰氧基-2-甲基-2-丁烯-1-醛。
이이무이희위원료,여삼록이청뇨산발생록순화반응,생성1,2가성화1,4가성산물혼합물,가성산물혼합물재농류산위최화제적조건하여을산항발생지화반응,지화결속후직접승온진행전위반응생성1-을선양기-4-록-3-갑기-2-정희。지후재복합최화제린산경이갑、린산이경갑화이갑기아풍적조건하,용TEMPO양화위목표산물4-을선양기-2-갑기-2-정희-1-철。
Using isoprene methyl butane as starting material in the chlorohydrination with trichloroiminocyanuric acid, 1, 2 and 1, 4-addition production mixture was formed.Following in the presence of concentrated sulfuric acid and esterification with acetic anhydride , heating directly for rearrangement , 1-acetoxy-4-chloro-3-methyl-2-butene was obtained.Using dipotassium phosphate , potassium dihydrogen phosphate and DMSO as complexing catalyst , desired product 4-acetoxy-2-methyl-2-butenal was synthesized by oxidation with TEMPO.