Synthesis and Crystal Structure of 2-Amino-5,6-dihydro-4-(3,4-dimethoxyphenyl)-4H-benzo[h]chromene-3-carbonitrile

The title compound 2-amino-5,6-dihydro-4-（3,4-dimethoxyphenyl）-4H-benzo[h]- chromene-3-carbonitrile （C22H20N2O3, Mr = 360.40） was obtained by the reaction of 2-（3,4-dimeth- oxybenzylidene）-1-tetralone and malononitrile in DMF in the presence of KF-montmorillonite. Its structure was confirmed by IR and ^1H NMR spectra. The crystal is of monoclinic, space group C2/c with a = 24.101（6）, b = 9.146（2）, c = 17.238（3） ,A, β= 95.92（2）°, Z = 8, V= 3779.4（14） ,A^3, Dc = 1.267 g/cm^3, μ（MoKa） = 0.085 mm^-1, F（000） = 1520, R = 0.0409 and wR = 0.0981 for 2043 observed reflections （I 〉 2σ（I））.

Synthesis and Crystal Structure of 4-(4-Chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydropyrimidin-2(H)-one

The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.

Synthesis and Crystal Structure of 1,3-Trans-1,4-cis- 3,4-di(4-bromophenyl)-1',2',3'-trihydro-1-hydroxy- benzo[g]bicyclo[3.3]octane-2-spiro-2'-indene-1'-one

The title compound C35H30Br2O3 （C32H24Br2O2·CH3COCH3） has been synthesized by the dimerization of 2-（4＇-bromobenzal）-1-indenone induced by low-valent titanium reagent, and characterized by elemental analysis, IR,^1H NMR and X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.273（7）, b = 11.036（7）, c = 13.944（9） ,A°, a = 73.972（9）, β =76.577（10）,γ= 88.871（10）°, V = 1476.3（17）A°^3, Mr = 658.41, Z = 2, Dr = 1.481 g/cm^3, μ（MoKa） = 2.780 mm^-1, F（000） = 668, the final R = 0.0452 and wR = 0.0975. X-ray analysis reveals that the two cyclopentane rings spiro-fused each other adopt envelope conformations, while the other cyclopentane ring （C（1）--C（2）-C（7）-C（9）） is coplanar. In addition, there is a classical intermolecular hydrogen bond O（1）-H（1）...O（2） connecting the adjacent molecules into dimers.

Synthesis and Crystal Structure of 1-(4-Chlorophenyl)-2-cyano-3-amino-3a-hydroxy- 3a,3b,6,7-tetrahydrobenzo[4,5]indene

The title compound 1-（4-chlorophenyl）-2-cyano-3-amino-3a-hydroxy-3a,3b,6,7- tetrahydro-benzo[4,5]indene 2, has been synthesized by the reductive cyclization of 2-cyano-3- （4-chlorophenyl）-3-（1-tetralon-2-yl） propionitrile 1 induced by low-valent titanium reagent and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group C2/c with a = 28.244（7）, b = 14.401（3）, c = 21.245（3）A,β= 115.71（2）°, V = 7786（3）A^3, Mr= 696.13, Dc = 1.188 g/cm^3, Z = 8,μ（MoKα） = 0.208 mm^-1, F（000） = 2916, R = 0.0783 and wR = 0.2350. X-ray analysis reveals that the five-membered ring （C（7）～C（l l）） adopts an envelop conformation, while the six-membered ring （C（10）～C（14）, C（19）） has a half-chair conformation. Meanwhile, intermolecular H-bond interactions result in the formation of polymer.

One-pot Synthesis of 3,4-Dihydropyrimidin-2(1H)-one Using TsOH as a Catalyst under Microwave Irradiation

A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 carbonyl compound and urea. The structure of 4o was determined by single crystal X ray diffraction analysis.

One-pot Synthesis of N-Hydroxylacridine Derivatives in Water

N-Hydroxylacridinedione derivatives were synthesized by three-component reaction of aromatic aldehydes, 1,3-dicarbonyl compounds and hydroxylamine hydrochloride using triethylbenzylammonium chloride （TEBA） as the catalysis in water. The reaction has many advantages including good yields, easy to be separated and environmental friendliness.

A Novel Reductive Cyclization of o-Nitrobenzamides and Ketones Promoted by Low-valent Titanium Reagent

A short and facile synthesis of a series of 1,2-dihydroquiazolin-4(3H)-ones was accomplished in good yields via novel reductive cyclization of o-nitrobenzamides with ketones promoted by TiCl4/Zn system. The structure was established on the basis of elemental analysis, IR, 1H NMR and confirmed by a single-crystal X-ray diffraction analysis. This method has the advantages of easily accessible starting materials, convenient manipulation and moderate to high yields.

An Efficient Method for the Synthesis of Indolo[3,2-c]quinoline Derivatives Catalyzed by Iodine

The reaction of Schiff base and indole catalyzed by iodine in DMA, subsequently treated with DDQ, gave indolo[3,2-c]quinoline derivatives in good yields. The structure of 3e was confirmed by X-ray diffraction analysis.