Synthesis and Crystal Structure of O,O-Dimethyl-N-(β-triphenylgermanyl)propionyl-α- aminobenzylphosphonates

The title compound (C30H32NO4PGe), O,O-dimethyl-N-(β-triphenylgermanyl) propionyl-α-aminobenzylphosphonates was synthesized by a convenient method, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is triclinic, space group P-1 with parameters: a=9.7753(5), b=11.5773(5), c=13.5059(6) ?, α=104.185(1),β= 95.971(1), γ =96.727(1)°, V=1457.63(12) ?3, Z=2, Mr=574.13, Dc=1.308 g/cm3, λ=0.71073 ?, μ = 1.139mm-1, and F(000)=596. The structure was solved by direct methods. The structure was refined to R=0.0257, wR=0.0705 for 5080 observed reflections with I >2σ(I).The result of structure analysis indicates that atom Ge is sp3 hydridized because the arrangement of the four carbon atoms bonded to it is a distorted tetrahedron. The geometry of the three phenyl groups linking with the Ge atom looks like a propeller form.

Investigation of Isomerization of 2-Seleno-1, 3, 2-diazaphospholidine Derivatives

For the first time the isomerization of 1, 3, 2-diazaphospholidine-2-selenide derivatives in refluxing benzene in the presence of trace water was observed. The structures of isomerized products were determined by IR, 1H NMR, 31P NMR, elemental analysis and X-ray crystallography. The mechanism of isomerization was also proposed.

A New Convenient Method for the Resolution of 1, 1'-Binaphthalene-2, 2'-diol Via a Phosphite Using (-)-Menthol as Resolving Agent

Menthol reacts with phosphorus trichloride to afford menthyl phosphorodichloridite 2, which further reacts with racemic 1, 1-binaphthalene-2, 2-diol to give phosphite (+)-3 in the presence of triethylamine. (+)-3 can be easily separated by fractional crystallization to form the crystal (+)-(S)-3 and the mother liquor (-)-(R)-3. Then both the crystal and the mother liquor are treated with AcOH-H2O to obtain enantiomeric pure (-)-(S)-1 and (+)-(R)-1 respectively, with enantiomeric excess up to 99.7%.

A Novel Fused Phosphorus Heterocycle: 4-(1',2',3',4-Tetrahydro-1, 3, 2-benzodiazaphosphorin-2'-sulfide)-3, 4b, 4a-thiazphosphaphenanthridine Derivative

The first example of fused phosphorus heterocyclic 4-[1-(b-bromoethyl)-4-oxo-3-prop yl-1, 2, 3, 4-tetrahydro-1, 3, 2-benzodiazaphosphorin-2-sulfide]-1, 2, 3, 4, 4a, 4b, 5, 6-octahydro -6-oxo-5-propyl-3, 4b, 4a-thiazphosphaphenanthridine 4a, 2-dioxide was synthesized in excellent yield by refluxing a mixture of 1-(2-bromoethyl)-2, 3-dihydro-3-propyl-1, 3, 2-benzodiazaphos phorin-4(1H)-one 2-oxide with carbon disulfide in benzene in the presence of triethylamine.

Synthesis and Reaction of [MnRe(CO)_6(μ-SH)(μ-SC(H)PPr_3~i)(PPh_3)]

The synthesis, the crystal structure and the reaction of the hetero-binuclear complex [MnRe(CO)6(-SH)(-SC(H)PPri3)(PPh3)] are reported. The results of single crystal X-ray structure analysis showed that the fragments Mn(CO)3 and Re(CO)3 were bridged by SH and SC(H)PPri3. The title complexes can react with BunLi and RX forming complexes MnRe(CO)6(-SR)(-SC(H)PPri3)(PPh3) (R = Me, CH2CH=CH2, SnBu3n).

Crystal and Molecular Structure of N,N-Bis(2-chloroethyl)-N'-isopropyl-N'-phenyl Thioureido Phosphoramide

The molecular structure of N, N-bis ( 2-chloroethyl )-N'-isopropyl-N'-phenyl thioureido phosphoramide has been determined by X-ray diffraction method. The crystal(C_14H_23Cl_4N_4OPS) is monoclinic with space group P21/n,α=13. 398(2) , b= 10. 351(4), c= 14. 595(3) A, β= 101. 45(1)°, V=1983(2) A3 Mr=397. 31, Z=4, Dx=1. 34 g/cm3 , μ= 5. 17 cm-1, F(000) = 832 , R=0. 056 and Rω=0. 060 for 1856 reflections with I≥3σ(Ⅰ).The chemical shifts of the hydrogen atoms bonded to nitrogen atoms N (4) and N (33 are 10. 96 ppm and 7. 57 ppm respectively locating in the lower field. This abnormal situation can be explained by the formation of intramolecular and intermolecular hydrogen bonds. And the X-ray crystallographic analysis demonstrates the existence of the H-bonding six-membered ring in the structure.

Crystal Structure of 3-[(α-Phenyl) triphenyl germylethyl]-4-phenyl -Δ￣2-1, 2, 4-triazoline-5-thione

The crystal structure of the title compound, C_34H_29GeN_3S, has been determined by single-crystal X-ray diffraction at 299 (±1)K. The crystal is trichlnic with space group P1, a=9. 772(3), b= 11. 643(3), c= 13. 960(3) A . α=66. 55(2),β=83. 49(2),γ=88. 49(2)°, Z=2, V= 1440. 0(8) A￣3, M_r=584. 28, F(000) =604, μ(MoKα) = 11. 44 cm￣-1. D_c= l. 349 g/cm￣-3. The final R factor is 0. 058, and R_w is 0. 068. The result of X-ray analysis indicates that the heterocycle of the title compound appears as a triazoline instead of a triazole.

Crystal Structure of 3-(4'-Methoxyl)-phenyl-5-cyano-6-methylthio Pyrimidine-2, 4-diones

The crystal of the title compound, 3-(4′-Methoxyl)-phenyl-5-cyano-6-methylthio pyrimidine-2, 4-diones, ([C13H11N3O3S]2, Mr=578.62)，has been prepared and determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with parameters: a = 11.602(2), b = 15.921(3), c = 13.918(3)?, ( = 94.38(3)(, V = 2563(1) ?3, Z = 4, Dc = 1.499g/cm3, μ(MoK()= 2.64cm-1, F(000)=1200. R and Rw are 0.054 and 0.059, respectively, for 1692 observed unique reflections. The pyrimidione ring is six-membered plane, and the dihedral angle between the pyrimidione ring and benzene ring is 121.05(. From the above result, it could be predicted that the negative atoms among the title compound might interact with target D1 protein, and thus express its inhibitory activity.

Crystal Structure of 1,2:5,6-Di-O-isopropylidene-α-D-glucofuranosyl N,N-bis(2-chloroethyl) Phosphordiamidate

The title compound,1,2:5,6 di-O-isopropylidene-α-D-glucofuranosyl N,N-bis(2-chloroethyl) N'-isopropylphosphordiamidate(C19H35O7N2PCl2),was synthesized by a series of reactions, and its crystal structure was determined by single crystal X-ray diffraction.The crystal is the orthorhombic space group P212121 with α=9. 996(3),b=22.149(5),c=11.858(3)A,V=2647.4A,Mr=505.4,Z=4,Dx=1.27 g/cm3, μ=3.4 cm-1,and F(000)=1080.The structure was solved by direct methods(SHELXS 86).The final refinement converged with unweighted and weighted agreement factors of 0.068 and 0. 072 for 2230 observed independent reflections with I≥3σ(I).The results of structure analysis indicate that the configuration of the chiral phosphorus atom is R-form.

Crystal Structure of Ethyl Ester N-(Isopropylcarbamoyl-Methoxyphosphonyl)-(1) -α-Phenylalanine

The title compound, ethyl ester N-(iso-propylcarbamoylmethoxyphosphonyl)-(1)-α-phenylalanine(C_16H_25N_2O_5P), was synthesized by a series of reactions, and its crystal structure was determined by single crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P2_1, with a=5. 256(1), b=15. 869(3) , c=11. 718(4) A. β=96. 50(3), V=971. 1(9) A￣3, M_r=356. 36,Z=2, D_c=1. 219 g/cm￣3, μ=0. 161 mm￣(-1), and F(000)=190. The final agreement factors are R=0. 057 and R_w=0. 055 for 1311 observed independent reflections with I ≥3σ(I). The results of structure analysis indicate that the configuration of the chiral phosphorus atom is S-form.