摘要
微波辐射下,在水溶液中以KOH催化苯酚与六氟丙酮三水合物(HFA·3H2O)的缩合反应,制备了2-(4-羟基苯基)六氟异丙醇的异构体混合物;目标产物结构经IR、1H NMR和MS确认。结果表明,与传统加热法相比,微波辐射法可明显缩短反应时间。在n(苯酚)∶n(HFA·3H2O)∶n(KOH)=3.0∶1.0∶0.3及微波功率为300 W条件下,反应时间可由常规加热法的35 h缩短至6 h,总收率由87%提高到90%,目标物产物选择性为94%。
With the assistance of microwave, a mixture of 2- （4-hydroxy-phenyl） -1,1,1,3,3,3-hexafluoro- propan-2-ol isomers were obtained via the condensation between hexafluoroacetone trihydrate（ HFA-3H20） and phenol using potassium hydroxide as catalyst. The product was characterized by ~H NMR, IR and MS spectra. The results show that the microwave-assisted process can reduce the reaction time remarkably compared with conventional processes. Under optimal conditions with the microwave power 300 W at n（phenol）：n（HFA-3H20）：n（KOH） =3.0：1.0：0.3, the reaction time are shortened from 35 h in conventional heating to 6 h, the total yield is increased from 87% to 90% with 94% selectivity.
出处
《应用化学》
CAS
CSCD
北大核心
2013年第12期1438-1442,共5页
Chinese Journal of Applied Chemistry
关键词
(羟基苯基)六氟异丙醇
苯酚
微波
氢氧化钾
六氟丙酮三水合物
正交实验法
（hydroxy-phenyl） -hexafluoro-propan-ol, phenol, microwave, potassium hydroxide, hexafluoroacetonetrihydrate, orthogonal experimental design
