摘要
以3-(3-叔丁基-4-羟基-5-甲基苯基)-丙酸甲酯(KY-250)与3,9-双(1,1-二甲基-2-羟基乙基)-2,4,8,10-四氧杂螺环[5.5]十一烷(螺环二醇)为原料,有机锡为催化剂,采用酯交换法在常压下合成了抗氧剂3,9-双{2-[3-(3-叔丁基-4-羟基-5甲基苯基)丙烯酸]-1,1-二甲基)-2,4,8,10-四氧杂螺环[5.5]十一烷(AO-80),产物结构经IR和核磁共振(~1H NMR,^(13)C NMR)进行了确证。较佳合成条件为:反应时间8 h,反应温度190℃,n (KY-250):n(螺环二醇):n(有机锡)=2.2:1:0.044。适宜的重结晶溶剂是w(CH_3OH)=9O%的甲醇溶液,与粗产物的质量比为7:1,收率为72%,产物质量分数大于99.6%。
3,9-Bis{ 2-[3-（3-tert-butyl-4-hydroxy-5-methylphenyl）-propionyloxy]-1, 1-dimethyl }-2,4,8, 10-tetraoxaspiro[ 5. 5 ] undecane （AO-80） was synthesized using methyl 3-（3-tert-butyl-4-hydroxy-5- methylphenyl） propionate（KY-250） and 3,9-bis（1,1-dimethyl- 2-hydroxyethyl）-2, 4,8,10-tetraoxaspiro[5.5]undecane （spiroglycol） as starting materials and organotin as catalyst by transesterification. The obtained optimal reaction conditions were., reaction time 8 h, reaction temperature 190 ℃, n（KY- 250） ： n（spiroglycol） ： n（organotin）=2.2 ： 1 ： 0. 044. The product was purified by recrystallization. The suitable solvent for the recrystalization was 90% methanol and the mass ratios of methanol to crude AO-80 were 7 ： 1. Under above conditions, the yield and purity of the product were ≥72% and ≥99. 6%, respectively. The structure of the product was characterized by IR, ^1H NMR and ^13 C NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2007年第4期7-9,共3页
Speciality Petrochemicals
