α-苯基丙酸的相转移催化合成

以苯乙酸为原料,相转移催化合成α-苯基丙酸。通过正交设计选出最佳实验条件,产品纯度在98%以上,收率达94%。

Co_2(CO)_8催化苯乙烯氢酯基化制α-苯基丙酸酯研究

以Co2(CO)8为催化剂,对苯乙烯与CO及甲醇氢酯基化反应制α-苯基丙酸甲酯的反应进行了研究,并根据实验结果提出了可能的催化反应机理.考察了催化剂用量、配体、溶剂、CO压力及反应温度等因素对氢酯基化反应的影响.结果表明:以甲苯为溶剂,在n(Co2(CO)8)/n(苯乙烯)=0.06,吡啶为配体且n(吡啶)/n(Co)=2,CO压力6.0 MPa、反应温度95℃的较佳条件下反应12 h,苯乙烯的转化率接近100%,α-苯基丙酸甲酯的收率达到89.07%,异正比24.35.

β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯/冰片酯合成研究

以3,4-二羟基苯甲醛为起始原料,经苄基保护、Darzens环氧化、Lewis酸开环、NaBH4还原、催化加氢脱保护得到β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯和β-(3,4-二羟基苯基)-α-羟基丙酸冰片酯,所得化合物的结构通过1HNMR、13CNMR,IR,MS证实.该方法操作简单、毒性低、产物易于纯化.

Synthesis and Crystal Structure of O,O-Dimethyl-N-(β-triphenylgermanyl)propionyl-α- aminobenzylphosphonates

The title compound (C30H32NO4PGe), O,O-dimethyl-N-(β-triphenylgermanyl) propionyl-α-aminobenzylphosphonates was synthesized by a convenient method, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is triclinic, space group P-1 with parameters: a=9.7753(5), b=11.5773(5), c=13.5059(6) ?, α=104.185(1),β= 95.971(1), γ =96.727(1)°, V=1457.63(12) ?3, Z=2, Mr=574.13, Dc=1.308 g/cm3, λ=0.71073 ?, μ = 1.139mm-1, and F(000)=596. The structure was solved by direct methods. The structure was refined to R=0.0257, wR=0.0705 for 5080 observed reflections with I >2σ(I).The result of structure analysis indicates that atom Ge is sp3 hydridized because the arrangement of the four carbon atoms bonded to it is a distorted tetrahedron. The geometry of the three phenyl groups linking with the Ge atom looks like a propeller form.

β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯滴丸制剂处方优化

目的:优化β-(3,4-二羟基苯基)-α-羟基丙酸异丙酯(IDHP)滴丸的制剂处方。方法:采用Box-Behnken中心组合设计,以载药量、淀粉用量和羧甲基淀粉钠用量为自变量,总评归一化值(OD)为因变量,利用响应曲面法分析自变量对因变量的影响,确定滴丸剂较优处方并进行验证。结果:IDHP滴丸的最佳处方为:载药量为23.0%,淀粉用量为14.0%,CMS-Na用量为4.0%,PEG6000用量为59.0%。结论:试验所得处方合理,IDHP滴丸的成型质量良好。