2,5-Dimethyl-4-phenyl- and 3,6-dimethyl-2,4-diphenylpiperidines

2,5-Dimethyl-4-phenylpiperidine and 3,6-dimethyl-2,4-diphenylpiperidine were obtained by reduction of the corresponding substituted pyridines. Several of their transformations are examined.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1356–1358, October, 1970.     

Synthesis and Crystal Structure of 3-Benzoyl-7,7-dimethyl-4-phenyl-2-phenylamino-4,6,7,8-tetrahydro-chromen-5-one

The title compound (C30H27NO3) was synthesized via a one-pot procedure starting from β-benzoylthioacetanilide, benzaldehyde and 5,5-dimethyl-1,3-cyclohexanedione, and its struc- ture was determined by single-crystal X-ray diffraction analysis. The crystal belongs to triclinic system, space group P, with a = 6.325(2), b = 11.243(3), c = 17.553(4) , α = 87.306(4), β = 80.822(4), γ = 77.798(4)°, V = 1204.2(5) 3, Z = 2, Mr = 449.53, Dc = 1.240 g/cm3, μ = 0.080 mm-1, F(000) = 476, the final R = 0.0459 and wR = 0.0970 for 2301 observed reflections with I > 2σ(I).     

Synthesis of 4-Amino-6-phenyl-3-thioxo-2,3-dihydro-1,2,4-triazine-5(4H)-one

Russian Journal of General Chemistry -     

Steric Structure of Bis(5,5-dimethyl-3-thioxo-1-cyclohexenyl) Sulfide

Two-dimensional NMR spectroscopy, dipole moment measurements, and quantum-chemical calculations (basis 6-31G^*) were used to show that in the gas phase and in solutions bis(5,5-dimethyl-3-thioxo-1-cyclohexenyl) sulfide prefers a nonplanar cis-trans conformation.     

微波辐照下4-苯基-7,7-二甲基-2,5-二氧代-1,2,3,4,5,6,7,8八氢喹啉的合成和晶体结构

标题化合物C1 7H1 9NO2 是由苯甲醛、5,5 二甲基 1 ,3 环己二酮、丙二酸亚异丙酯及醋酸铵在微波辐照下干反应而得。结构通过单晶X 射线衍射法确定 ,其晶体属于单斜晶系 ,空间群P2 1 /a ,a =7.52 4 (2 ) ,b =2 2 .483(3) ,c =9.2 73(2 ) ,β =1 1 3 0 4 (2 )°,V =1 44 3.7(5) 3,Mr=2 69.34,Dc=1 .2 39g/cm3,Z =4,μ(MoKα) =0 81cm- 1 ,F(0 0 0 ) =576,在 6 <2θ <51 0°范围内收集 2 994个独立衍射点 ,其中可观测衍射点 2 0 91个 [I >2 .50σ(I) ]。晶体结构用直接法解出 ,经用全矩阵最小二乘法对原子参数进行修正 ,最后的偏离因子为R =0 .0 4 4 ,Rw=0 .0 58。在晶体结构中 ,O(3) -C(9) -C(4) -C(5) -N(1 )构成一个平面 ,该平面与苯环的二面角为 84.2 5°     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.     

2,3,6,7,8,9-hexahydro-8,8-dimethyl-5-phenyl-1-H1,4-benzodiazepin-6-one

Several approaches for the synthesis of the title compound 1 were investigated. Treatment of the ethane-1,2-diamine derivative 2 with phosphoryl chloride afforded 3-chloro-5,5-dimethylcyclohex-2-enone (3) and 1-(5,5-dimethyl-3-oxocyclohex-1-enyl)-4,5-dihydro-2-phenylimidazole (4) , The reaction of 2-benzoyl-dimedone (5) with an equimolar amount of ethane-1,2-diamine led to the 2:1 adduct 6 , whereas with an excess of ethane-1,2-diamine, 4,5-dihydro-2-phenylimidazole (7) and dimedone were obtained. The synthesis of the title compound 1 was achieved by reacting 2-benzoyl-3-chloro-5,5-dimethylcyclohex-2-enone (8) with ethane-1,2-diamine.     

Tautomerism in 1-phenyl-3-carbomethoxyphosphorinan-4-one and its derivatives

Conclusions The possibility is discussed of using tautomerism to determine the conformational free energies of ring substituents, and the free energy of steric interaction of the substituents in the individual stereoisomers of 1-phenyl-3-carbomethoxyphosphorinan-4-one and its derivatives.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 7, pp. 1533–1540, July, 1978.