微波辐射下2-氨基-7,7-二甲基-3-乙氧羰基- 4-(2-呋喃)基-5-氧代-5,6,7,8-四氢-4H- 苯并吡喃的合成和晶体结构

标题化合物C18H21NO5是由2-呋喃亚甲叉氰乙酸酯和5,5-二甲基-1,3-环己酮在醋酸铵存在下用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属三斜晶系,空间群P 睿琈r =332.36,a =11.232(2),b =13.048(2),c =13.274(3),α=105.7(1),β=95.68(2),g =109.56(1)? V=1752.4(6)3,Z=2,Dc=1.276Mg·m-1, =0.093mm-1,F(000)=704, 最终的偏离因子为R=0.0431,wR=0.0973,在分子结构中平面 1 (呋喃环) 与平面2 ((C(5)、 C(6)、C(9)、O(1))之间的二面角为 84.70°, 平面2 与平面 3 (C(1)、C(4)、C(5)、C(6)) 之间的二面角为 2.9°, 平面 1 与平面3 之间的二面角为 85.9°。吡喃环和与吡喃环合的六员环为信封式结构。

Synthesis and Crystal Structure of 2-Amino-7,7-dimethyl-3-toehxycarbonyl-4-(2-furyl)-5-oxo-5,6,7,8-tetrahydro-4-H-benzo-[b]-pyran under Microwave Irradiation

The title compound (C18H21NO5) has been synthesized by the reaction of 2-furyldenealdehyde ethyl cyanoacetoacetate with 5,5-dimethyl-1, 3-cyclohexanedione under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is triclinic, space group P with a=11.232(2), b=13.048(2), c=13.274(3)? =105.730(1), =95.68(2), = 109.560(1)? V=1725.4(6)?, Z=2, Mr=332.36, Dc=1.276g/cm3, (MoK?=0.083mm-1, F(000)=704. The structure was solved by direct methods and refined by full-matrix least squares-method to the final R=0.0431, wR=0.0973. X-ray analysis reveals that the dihedral angle between plane 1(furan) and plane 2(C(5) C(6) C(9) O(1)) is 84.70? between plan 2 and plan 3 (C(1) C(4) C(5) C(6)) is 2.9? between plan 1 and plan 3 is 85.9? the pyran cycle and the six-membered cycle fused with it are of envelope configurations in the structure.