Visible-light-initiated tandem synthesis of difluoromethylated oxindoles in 2-MeTHF under additive-,metal catalyst-,external photosensitizer-free and mild conditions

An efficient and eco-friendly protocol for synthesizing difluoromethylated oxindoles through a visiblelight induced one-pot tandem reaction of N-arylacrylamides,difluoroacetic acid and Ph I(OAc)_(2)was developed.This reaction proceeded in the absence of any additive,base,metal-catalyst and external photosensitizer,using cheap and easily available CHF_(2)CO_(2)H as the difluoromethylation reagent and bulk biomass-derived 2-Me THF as the sole solvent.26 Examples of N-arylacrylamide substrates were investigated,and all of them successfully underwent difluoromethylation to deliver the target products in good to excellent yields.

超细Cu/Ni催化糠醛加氢合成2-甲基四氢呋喃

采用溶胶凝胶法制备了超细Cu/Ni混合催化剂,并用于糠醛液相加氢制2-甲基四氢呋喃(2-MeTHF)反应。考察了Cu/Ni摩尔比、Na2CO3溶液浓度等对催化剂制备的影响,及反应压力、反应温度、反应时间等对糠醛转化率和2-MeTHF选择性的影响。结果表明,适宜催化剂制备条件为n(Cu)∶n(Ni)=1∶1,Na2CO3溶液浓度为1.0mol/L;适宜的反应条件为反应压力8 MPa,反应时间3.5 h,反应温度180℃;产品经气相色谱检测分析,糠醛的转化率为100%,2-MeTHF的选择性为64.52%。

PVA/PVP共混交联膜对2-甲基四氢呋喃溶液渗透汽化脱水的研究

利用共混交联法将马来酸酐(MAH)加入聚乙烯醇(PVA)和聚乙烯吡咯烷酮(PVP)混合溶液中制备PVA/PVP膜。考察了膜的组成、料液中水质量分数和温度对渗透汽化分离性能的影响。结果表明,在V(PVA)∶V(PVP)=8∶2、水质量分数为3.9%的2-甲基四氢呋喃(2-Me THF)溶液和最佳温度为68℃条件下,渗透通量和分离因子分别可达431.64 g/(m^(2)·h)和272.96。PVA/PVP膜能有效分离2-Me THF/水溶液。SEM、XRD、接触角、机械强度分析结果表明,交联后的PVA/PVP膜均匀致密,结晶度、水接触角明显降低,机械强度显著增强。

头孢地尼的绿色合成工艺

用乙酰基替代三苯甲基保护去甲氨噻肟酸乙酯中的肟羟基,使头孢地尼活性酯与7-AVCA的缩合反应和肟羟基的去保护反应合二为一;用绿色溶剂2-甲基四氢呋喃替代二氯甲烷,应用于头孢地尼的合成;将副产物三苯基氧膦和2-巯基并噻唑回收并再生为三苯基膦和DM,循环利用,从源头上减少了三废排放量,具有工业化应用前景。