摘要
以2,2-二甲基-3-(2-氯-3,3,3-三氟-1-丙烯基)环丙烷甲酸为起始原料,经酰氯化、胺基化、羟甲基化反应,合成了2,2-二甲基-3-(2-氯-3,3,3-三氟-1-丙烯基)-N-羟甲基环丙烷甲酰胺.目标产物经IR,1HNMR,MS,元素分析测定其组成和结构,其晶体结构经X-ray衍射仪测定,晶体属于单晶斜系,P21/c空间群,a=1.879 6(4)nm,b=0.711 34(13)nm,c=2.460 9(4)nm,α=90°,β=129.390(10)°,γ=90°,V=2.542 9(9)nm3,Z=8,DC=1.419 mg/m3,F(000)=1 120,μ=0.327 mm-1,可观测点精修最终偏离因子R1=0.141 5,wR2=0.487 4.
3-( 2-chloro-3, 3, 3-trifluoroprop 1-enyl)-N-hydroxymethyl-2, 2-dimethylcyclopropanecarboxarnide was synthesized from 2,2-dimethyl-3- (2,2-chloro-3,3,3-trifluoro- 1-propenyl) cyclopropanecarboxylic acid by acylation, amidogen and hydroxymethyled reactions. The structure of the product was confirmed by elemental analysis, IR, 1H NMR and MS. The crystal structure of the product was determined by X-ray diffraction analysis. The product belongs to the monoclinic system with space group P21/c, a=1. 879 6(4) nm, b=0. 711 34(13) nm, c=2. 460 9(4) nm, a =90°, β=129.390(10)°, γ=90°, V=2.542 9(9) nm^3, Z=8, Dc=1.419 mg/m^3, F(000)= 1 120, μ=0. 327 mm^-1 , the final R1 =0. 141 5, wR2=0. 487 4.
出处
《浙江工业大学学报》
CAS
2008年第3期268-271,共4页
Journal of Zhejiang University of Technology