The title compound(9S,13R,14S)-7,8-dehydro-4-(4'-bromo-benzyloxy)-3,7-dime-thoxy-17-methyl-morphinan-6-one monohydrate(O-4-bromobenzylsinomenine) was synthesized by the reaction of(9S,13R,14S)-7,8-dehydro-4-hydroxy-3,7-dimethoxy-17-methyl-morphinan-6-one with 4-bromobenzyl alcohol.Its chemical structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21 with a = 8.890(2),b = 14.757(4),c = 9.205(2) ,β = 91.577(4)°,C26H30BrNO5,Mr = 516.42,μ = 1.740 mm-1,V = 1207.2(5)3,Z = 2,Dc = 1.421 mg/m3,F(000) = 536,R = 0.0785 and wR = 0.1889.
Poly(L-lactide-co-caprolactone)(85-15)[P(LLA-CL)(85-15)] was synthesized from high purity L-lactide and ε-caprolactone using tin octoate as initiator by ring-opening polymerization, and characterized by infrared spectrum and 1H-NMR spectrum. The synthesized P(LLA-CL)(85-15) is a random copolymer. The influences of polymerization temperature, polymerization time, dosage of initiator and polymerization pressure on the weight average molecular weight and the polydispersity index of P(LLA-CL)(85-15) were investigated. The optimum preparation conditions of P(LLA-CL)(85-15) are: the polymerization pressure is less than 0.5 Pa, the polymerization temperature is 130 ℃, the n(M)/n(I) ratio is 8 000/1, and the polymerization time is 36 h. Under the condition, the weight-average molecular weight of prepared P(LLA-CL)(85-15) is 65.6×104, and molecular weight distribution coefficient is 1.15.
Gas chromatography-mass spectrometry(GC-MS) and the chemometric resolution method(alternative moving window factor analysis,AMWFA) were used for comparative analysis of volatile constituents in herbal pair(HP) flos lonicerae-caulis lonicerae(FL-CL) and its single herbs.The temperature-programmed retention index(PTRI) was also employed for the identification of compounds.In total,44,39,and 50 volatile chemical components in volatile oil of FL,CL and HP FL-CL were separately determined qualitatively and quantitatively,accounting for 87.22%,94.54% and 90.08% total contents of volatile oil of FL,CL and HP FL-CL,respectively.The results show that there are 32 common volatile constituents between HP FL-CL and single herb FL,33 common volatile constituents between HP FL-CL and single herb CL,and 10 new constituents in the volatile oil of HP FL-CL.
The title compound (7R,8S,9S,12S)-13,14-dehydro-1-(4-fluorobenzyloxy)-N-methyl-2,13-dimethoxy-12-hydroxymorphinane was synthesized by the reaction of O-4-bromobenzyl-sinomenine with lithium aluminum hydride.Its chemical structure was determined by X-ray single-crystal diffraction.The crystal belongs to triclinic,space group P1 with M r=439.51,a=7.7236(1),b=8.7282(1),c=9.9342(2),α=81.176(1),β=67.43,γ=64.577(1)°,μ=0.76 mm-1,V=558.45(2)3,Z=1,D c=1.307 mg/m 3,F(000)=234 and T=133 K.
