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以1,1-二苯基-1-[(2S,4R)-4-(4-乙烯基-苄氧基)-2-吡咯烷基]-甲醇(Ⅱ)为功能性单体,经苯乙烯共聚、二乙烯苯交联后与甲基硼酸进行缩合反应,制备了大孔树脂支载的CBS(手性口恶唑硼烷类化合物)催化剂(Ⅳ),并应用于催化苯乙酮不对称还原反应。利用红外光谱对催化剂Ⅳ进行了表征,并考察了交联度、功能性单体摩尔分数及催化剂的循环使用性能对催化反应的影响。还原产物(R)-1-苯乙醇(Ⅵ)采用红外、核磁共振(1HNMR、13CNMR)进行了结构表征。对催化剂在自建的连续反应装置上的催化性能进行了评价。结果表明:当支载催化剂的交联度为8%,功能性单体摩尔分数为9.67%时,连续催化苯乙酮不对称还原为(R)-1-苯乙醇的转化率接近100%,ee(对映体过量)值接近90%。催化剂连续使用25 h后,ee值没有降低的趋势。
Using 1,1-diphenyl-1 - [(2S, 4R) -4- (4-vinyl- benzyloxy) -2-pyrrolidinyl] -methanol (II) as functional monomer, Ethylene copolymer and divinylbenzene were cross-linked with methyl boric acid to prepare a macroporous resin supported CBS (chiral oxazaborolidine) catalyst (Ⅳ), and applied to the catalytic acetophenone not Symmetrical reduction reaction. The catalyst IV was characterized by FTIR, and the influence of the degree of crosslinking, the mole fraction of functional monomer and the cyclic performance of the catalyst on the catalytic reaction were investigated. The reduction product (R) -1-phenylethanol (Ⅵ) has been characterized by IR and 1HNMR (13CNMR). The catalytic performance of the catalyst on a self-built continuous reactor was evaluated. The results showed that the conversion of acetophenone to (R) -1-phenylethanol was nearly 100% when the degree of crosslinking of supported catalyst was 8% and the molar fraction of functional monomer was 9.67% The ee (enantiomeric excess) value is close to 90%. After continuous use of catalyst for 25 h, the ee value did not decrease.