西北大学学报（自然科学版）
西北大學學報（自然科學版）
서북대학학보（자연과학판）
JOURNAL OF NORTHWEST UNIVERSITY(NATURAL SCIENCE EDITION)
2010年
1期
81-84
,共4页
3,5-二氯4-氟三氟甲苯%3,4,5-三氯-三氟甲苯%TMSO_2%氟化反应%相转移催化
3,5-二氯4-氟三氟甲苯%3,4,5-三氯-三氟甲苯%TMSO_2%氟化反應%相轉移催化
3,5-이록4-불삼불갑분%3,4,5-삼록-삼불갑분%TMSO_2%불화반응%상전이최화
3,4,5 -trichloro-benzotrifluoride%3,5-dichloro-4-fluoro-triluorotoluene%TMSO_2%fluorination%phase transfer catalysis
目的 研究3,5-二氯4-氟三氟甲苯的合成工艺.方法 以3,4,5-三氯-三氟甲苯和氟化钾为原料通过相转移催化合成目标产物.结果 确定了反应的最佳条件为反应物物质的量比n(3,4,5-三氯-三氟甲苯):n(氟化钾)=1:1.5,催化剂与原料质量比m(PEG-600):m(原料)=0.5～0.7:100,原料与溶剂环丁砜(TMSO_2)体积比为1:3～3.5,190~195℃反应12 h,原料转化率大于87%,收率80%,产品纯度大于98%(质量分数).结论 为工业化生产3,5-二氯4-氟三氟甲苯提供了依据.
目的 研究3,5-二氯4-氟三氟甲苯的閤成工藝.方法 以3,4,5-三氯-三氟甲苯和氟化鉀為原料通過相轉移催化閤成目標產物.結果 確定瞭反應的最佳條件為反應物物質的量比n(3,4,5-三氯-三氟甲苯):n(氟化鉀)=1:1.5,催化劑與原料質量比m(PEG-600):m(原料)=0.5～0.7:100,原料與溶劑環丁砜(TMSO_2)體積比為1:3～3.5,190~195℃反應12 h,原料轉化率大于87%,收率80%,產品純度大于98%(質量分數).結論 為工業化生產3,5-二氯4-氟三氟甲苯提供瞭依據.
목적 연구3,5-이록4-불삼불갑분적합성공예.방법 이3,4,5-삼록-삼불갑분화불화갑위원료통과상전이최화합성목표산물.결과 학정료반응적최가조건위반응물물질적량비n(3,4,5-삼록-삼불갑분):n(불화갑)=1:1.5,최화제여원료질량비m(PEG-600):m(원료)=0.5～0.7:100,원료여용제배정풍(TMSO_2)체적비위1:3～3.5,190~195℃반응12 h,원료전화솔대우87%,수솔80%,산품순도대우98%(질량분수).결론 위공업화생산3,5-이록4-불삼불갑분제공료의거.
Aim To research the synthesis process of 3,5-dichloro-4-fluoro-trifluoro-toluene. Methods The title compound was synthesized from 3, 4, 5-dichloro-trifluoro-toluene and KF by phase transfer catalysis. Results Using TMSO_2 as solvent, mole ratio n (3 ,4,5-trichlorobenzotrifluride) : n (KF) = 1: 1. 5, weight ratio m(PEG-600)m(3,4,5-trichloro-benzotrifluoride) = 0. 5～ 0. 7: 100, volume ratio V(3, 4, 5-trichlorobenzotrifluoride) : V (TMSO_2) = 1: 3～3. 5, stirring for 12h at 190～195 ℃, the conversion of 3 ,4,5-trichlorobenzotrifluoride is 87% ,the yield is 80% , and the content is more than 98% . Conclusion The process was mild and available for synthesis of 3 , 5-dichloro-4-fluoro-trifluorotoluene.
