A series of five N,N-disubstituted acylguanidines R1C（O）N=C[N（H）R2]NR23（R1=Mes or Ph; R2=Ar′′or Ar′; R3=Cy, Bn, iPr, or Et）（Mes=2,4,6-Me3C6H2, Ar′′=2,6-iPr2C6H3, Ar′=2,6-Me2C6H3） was synthesized from the...A series of five N,N-disubstituted acylguanidines R1C（O）N=C[N（H）R2]NR23（R1=Mes or Ph; R2=Ar′′or Ar′; R3=Cy, Bn, iPr, or Et）（Mes=2,4,6-Me3C6H2, Ar′′=2,6-iPr2C6H3, Ar′=2,6-Me2C6H3） was synthesized from the reactions of parent acylthioureas with respective secondary amines. According to structutral characterization by single-crystal X-ray diffraction, the rough reduction of the steric hindrance of R substitutents of R1 C（O）N=C[N（H）R2]NR23（also abbreviated as R1-R2-R3 for comparison purposes） led to the slight enlongation of N（1）–C（1） bond lengthes and small decrease of N（1）–C（1）–N（3） bond angles from Mes–Ar′′–Cy（1） to Ph–Ar′′–Bn（2）, Ph–Ar′′–iPr（3） and Ph–Ar′–Cy（4）. At the same time, the N（1）–H（1）···O（1） intramolecular hydrogen bonds were observed in these cases. When R3=Et, an interesting compound Ph-Ar′-Et（5） was obtained with the formation of intermolecular hydrogen bonds instead. 1 belongs to the monoclinic system, space group P2（1/n） with a=9.6488（3）, b=28.5318（8）, c=11.9155（3） A, b=91.439（2）°, V=3279.27（16） A3, and Z=4. 2 belongs to the triclinic system, space group P1 with a=9.6759（7）, b=10.8613（8）, c=15.7642（12） A, a=70.429（3）, b=79.257（4）, g=69.052（4）°, V=1453.63（19） A3 and Z=2. 3 belongs to the monoclinic system, space group P2（1/c） with a=11.1393（4）, b=13.0643（4）, c=17.6600（6） A, b=101.866（2）o, V=2515.09（15） A3 and Z=4. 4 belongs to the monoclinic system, space group C2/c with a=17.8466（3）, b=13.6126（2）, c=21.6710（4） A, b=90.7310（10）°, V=4992.72（14） A3 and Z=8. 5 is of orthorhombic system, space group P212121 with a=10.5555（2）, b=11.8913（2）, c=14.9558（4） A, V=1877.23（5） A3 and Z=4.展开更多
基金supported by the National Natural Science Foundation of China(21771194)the Special Fund for Agro-scientific Research in the Public Interest(201503108)
文摘A series of five N,N-disubstituted acylguanidines R1C（O）N=C[N（H）R2]NR23（R1=Mes or Ph; R2=Ar′′or Ar′; R3=Cy, Bn, iPr, or Et）（Mes=2,4,6-Me3C6H2, Ar′′=2,6-iPr2C6H3, Ar′=2,6-Me2C6H3） was synthesized from the reactions of parent acylthioureas with respective secondary amines. According to structutral characterization by single-crystal X-ray diffraction, the rough reduction of the steric hindrance of R substitutents of R1 C（O）N=C[N（H）R2]NR23（also abbreviated as R1-R2-R3 for comparison purposes） led to the slight enlongation of N（1）–C（1） bond lengthes and small decrease of N（1）–C（1）–N（3） bond angles from Mes–Ar′′–Cy（1） to Ph–Ar′′–Bn（2）, Ph–Ar′′–iPr（3） and Ph–Ar′–Cy（4）. At the same time, the N（1）–H（1）···O（1） intramolecular hydrogen bonds were observed in these cases. When R3=Et, an interesting compound Ph-Ar′-Et（5） was obtained with the formation of intermolecular hydrogen bonds instead. 1 belongs to the monoclinic system, space group P2（1/n） with a=9.6488（3）, b=28.5318（8）, c=11.9155（3） A, b=91.439（2）°, V=3279.27（16） A3, and Z=4. 2 belongs to the triclinic system, space group P1 with a=9.6759（7）, b=10.8613（8）, c=15.7642（12） A, a=70.429（3）, b=79.257（4）, g=69.052（4）°, V=1453.63（19） A3 and Z=2. 3 belongs to the monoclinic system, space group P2（1/c） with a=11.1393（4）, b=13.0643（4）, c=17.6600（6） A, b=101.866（2）o, V=2515.09（15） A3 and Z=4. 4 belongs to the monoclinic system, space group C2/c with a=17.8466（3）, b=13.6126（2）, c=21.6710（4） A, b=90.7310（10）°, V=4992.72（14） A3 and Z=8. 5 is of orthorhombic system, space group P212121 with a=10.5555（2）, b=11.8913（2）, c=14.9558（4） A, V=1877.23（5） A3 and Z=4.
