CAJ | 학술논문

2-取代苯胺与巴豆醛反应合成了5种8-取代喹哪啶.讨论了反应因素对反应的影响,得到了较好的结果.8-取代喹哪啶的结构经1HNMR和MS分析确证,并用单晶X-射线衍射测定了化合物Ⅰa和Ⅰb的晶体结构.化合物Ⅰa晶体属正交晶系,空间群为Pca2_1,晶胞参数为:a = 1.279 61(9) nm,b= 0.506 60(4) nm, c = 1.311 81(9) nm,Z = 4,V=0.850 38(11) nm~3, D_c = 1.387 g/cm~3, F(000)= 368, R_1 = 0.028 8, wR_2 = 0.073 1,S = 1.01;化合物Ⅰb晶体属单斜晶系,空间群为P2_1/c晶胞参数为:a = 0.504 40(17) nm,b = 1.346 7(4) nm, c = 1.339 1(4) nm, β = 97.678(4)°;Z = 4,V =0. 901 4(5) nm~3, D_c = 1.636 g/cm~3,F(000)= 440,R_1= 0.071 1, wR_2 = 0.195 1,S = 1.09. 选择合适溶剂和添加剂,反应收率较文献值有较大提高.
2-취대분알여파두철반응합성료5충8-취대규나정.토론료반응인소대반응적영향,득도료교호적결과.8-취대규나정적결구경1HNMR화MS분석학증,병용단정X-사선연사측정료화합물Ⅰa화Ⅰb적정체결구.화합물Ⅰa정체속정교정계,공간군위Pca2_1,정포삼수위:a = 1.279 61(9) nm,b= 0.506 60(4) nm, c = 1.311 81(9) nm,Z = 4,V=0.850 38(11) nm~3, D_c = 1.387 g/cm~3, F(000)= 368, R_1 = 0.028 8, wR_2 = 0.073 1,S = 1.01;화합물Ⅰb정체속단사정계,공간군위P2_1/c정포삼수위:a = 0.504 40(17) nm,b = 1.346 7(4) nm, c = 1.339 1(4) nm, β = 97.678(4)°;Z = 4,V =0. 901 4(5) nm~3, D_c = 1.636 g/cm~3,F(000)= 440,R_1= 0.071 1, wR_2 = 0.195 1,S = 1.09. 선택합괄용제화첨가제,반응수솔교문헌치유교대제고.
Five quinaldine derivatives were synthesized through the reaction of 2-substituted aniline and crotonaldehyde,and the effect of conditions on reaction were investigated. Their structure was confirmed by 1HNMR and MS. Crystal structure of Ⅰa and Ⅰb have been determined by X-ray diffraction. The compound Ⅰa crystal belongs to orthorhombic system with space group Pca2_1 and cell parameters: a = 1.279 61(9) nm, b = 0.506 60(4) nm, c = 1.311 81(9) nm, Z= 4,V= 0.85038(11) nm~3, D_c = 1.387 g/cm~3, F(000)= 368, R_1 = 0.028 8, wR_2 = 0.073 1,S = 1.01.The compound Ⅰb crystal belongs to monoclinic system with space group P2_1/c and cell parameters: a = 0.504 40(17) nm,b=1.3467(4) nm, c= 1.3391(4) nm, β= 97.678(4)°;Z = 4,V = 0.9014(5) nm~3, D_c=1.636 g/cm~3,F(000) = 440, R_1 = 0.071 1, wR_2 = 0.195 1,S=1.09.The yields of 8-substituted quinaldine are higher than that of literature by using appropriate slovent and additives.