摘要
根据Kornblum反应,采用二甲基亚砜(DMSO)氧化E-1-乙酰氧基-4-氯-3-甲基-2-丁烯(ACMB)合成E-4-乙酰氧基-2-甲基-2-丁烯-1-醛(AMBA)。在实验过程中,采用气相色谱跟踪,研究了反应时间、反应温度和催化剂用量等因素对主副产物收率的影响并确定了较佳反应条件:反应时间24 h,反应温度80℃,原料缓慢滴加,KH2PO4:K2HPO4:ACMB=0.14:1.27:1(摩尔比),催化剂用量与原料ACMB比为0.12:1(摩尔比)。同时,对从未报道过的副产物E-1-乙酰氧基-4-甲巯基-3-甲基-2-丁烯(AMMB)进行了结构鉴定,并推测了其形成机理。
E-4-acetoxy-2-methyl-2-buten-l-al was synthesized by oxidating E-l-acetoxy-4-chlorin-3-methyl-2-butylene with dimethylsulfoxide. The oxidation process was monitored by Gas-chroma-to-graphy. The effects of temperature, reaction time and the amount of the catalyst etc. to the yield of the main and side product were determined. The preferably conditions were ?reation time 24h, reation temperature 80℃, the raw material was added for 22 hours and reacted for more 2 hours , the mole proportion of the alleviant and catalyst to the raw material was KH2PO4 : K2HPO4: ACMB = 0.14 :1.27 : 1 , NaBr : ACMB=0.12 : 1 respectively. Simultaneously, the side product was identified, which was not identified yet, and the creation mechanism was presumed.
出处
《化学反应工程与工艺》
CAS
CSCD
北大核心
2004年第2期188-192,共5页
Chemical Reaction Engineering and Technology
