摘要
以对氯苯酚和3-氯丙酸为起始原料,在相转移催化剂三乙基苄基氯化铵催化下,合成对氯苯氧丙酸(1),然后用浓硫酸环化合成6-氯苯并二氢吡喃-4-酮(2)。考察了催化剂的用量、原料配比和反应时间对1收率的影响,适宜条件为:n(三乙基苄基氯化胺):n(对氯苯酚):n(3-氯丙酸):n(氢氧化钠)=0.023:1:1.3:1.3,反应时间为3h,收率为30.9%。此合成方法操作简便、安全、反应时间短且成本低。
A facile synthesis of 3,4-2H-6-chlorobenzopyran-4-one from the reaction of p-chlorophenol and 3- chloropropanoic acid via 4-chlorophenoxy propionic acid was reported with benzyhriethylammonium chloride (TEBAC) as the phase transfer catalyst. The title compound was obtained in 30.9% yield under the optimized conditions [ n (TEBAC) :n (p-chlorophenol) :n (3-chloropropanoic acid) :n (NaOH) = 0.023:1:1.3:1.3, t=3 h ].
出处
《精细化工中间体》
CAS
2010年第2期38-40,共3页
Fine Chemical Intermediates
基金
肇庆市科技计划创新(2009G12)资助项目