N‐(4‐Methyl­phenyl)‐N‐(5‐nitro­furfuryl)‐N‐prop‐2‐ynyl­amine

The title compound, C₁₅H₁₄N₂O₃, is the first example of a structurally determined tertiary amine with both N‐5‐nitro­furfuryl and N‐prop‐2‐ynyl moieties. The mol­ecule is not planar, i.e. the furan ring is inclined at an angle of 84.35 (4)° to the phenyl ring. The crystal structure is dominated by van der Waals forces. The terminal alkynyl group as the strongest C—H hydrogen‐bond donor is not involved in hydrogen‐bond formation.     

Hexanuclear Wheel‐Shaped Lithium N‐(2,6‐Diisopropylphenyl)‐N′‐(2‐pyridylethyl)benzamidinate

Lithiation of N‐(2,6‐diisopropylphenyl)‐N′‐(2‐pyridylethyl)benzamidine ( 1 ) with LiN(SiMe₃)₂ in a solvent mixture of toluene and TMEDA yields hexameric lithium N‐(2,6‐diisopropylphenyl)‐N′‐(2‐pyridylethyl)benzamidinate ( 2 ), which can be purified by recrystallization from a solvent mixture of toluene and THF. The three‐coordinate lithium ions have T‐shaped coordination spheres. The negative charge is delocalized within the 1,3‐diazaallylic system, which adopts a (syn‐Z)‐arrangement.     

N‐(4‐Methoxy­benzyl­idene)‐N′‐(2‐pyridyl)­hydrazine

Molecules of the title compound (alternative name p‐methoxybenzaldehyde 2‐pyridyl­hydrazone), C₁₃H₁₃N₃O, adopt an E configuration about the azomethine C=N double bond. Molecules are almost planar, the dihedral angle between the pyridine and methoxy­phenyl rings being only 6.19 (12)°. Pairwise N—H⃛N hydrogen bonds [R(8) in graph‐set notation] link centrosymmetrically related mol­ecules into discrete pairs.     

Synthesis of novel N‐alkyl/aryl‐N′‐(4‐arylthiazol‐2‐yl)‐N″‐xylosyl guanidines

The reaction of 2,3,4‐tri‐O‐acetyl‐β‐D‐xylopyranosyl isothiocyanate ( 1 ) and 2‐amino‐4‐arylthiazoles ( 2 ) gave xylosylthioureas 3 . These thiourea derivatives reacted with alkyl/aryl amine in the presence of HgCl₂ to give a new series of N‐alkyl/aryl‐N″‐(4‐arylthiazol‐2‐yl)‐N″‐xylosyl guanidines 4 . Some of the synthesized guanidines were screened for their biological activity. © 2007 Wiley Periodicals, Inc. Heteroatom Chem 18:688–694, 2007; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20379     

(2E)‐N‐(2‐Iodo‐4,6‐dimethylphenyl)‐2‐methylbut‐2‐enamide

The title compound, C₁₄H₁₈INO, crystallizes as +sc/+sp/+sc 2‐iodoanilide molecules (and racemic opposites) and shows significant intermolecular I...O interactions in the solid state, forming dimeric pairs about centres of symmetry. Under asymmetric Heck conditions, the S enantiomer of the dihydroindol‐2‐one was obtained using (R)‐(+)‐2,2′‐bis(diphenylphosphino)‐1,1′‐binaphthyl [(R)‐BINAP], suggesting a mechanism that proceeds by oxidative addition to give the title (P) enantiomer of the compound and pro‐S coordination of the Re face of the alkene in a conformation similar to that defined crystallographically, except that rotation about the C—C bond of the butenyl group is required.     

N‐(2‐Amino­benz­yl)‐N,N‐bis­(quinolin‐2‐ylmeth­yl)amine

The title new diquinaldine derivative, C₂₇H₂₄N₄, forms mol­ecular assemblies organized by inter­molecular quinoline π–π stacking [3.356 (3) and 3.440 (3) Å] and both inter‐ and intra­molecular N—H⋯N hydrogen bonds [3.039 (3)–3.104 (3) Å and 129 (2)–172 (2)°]. The combination of such inter­actions provides readily definable contacts that propagate along each crystallographic axis.     

A New Route to N‐Aryl 2‐Alkenamides,N‐Allyl N‐Aryl 2‐Alkenamides,and N‐Aryl α,β‐Unsaturated γ‐Lactams from N‐Aryl 3‐(Phenylsulfonyl)propanamides

A series of N‐aryl 2‐alkenamides were produced efficiently by treating N‐aryl 3‐(phenylsulfonyl)‐propanamides with potassium tert‐butoxide in THF at 0°C. With out isolation, it was further treated with an additional equivalent of potassium tert‐butoxide and allyl bromide to give N‐allyl N‐aryl 2‐alkenamides in one pot in good yields. Followed by a ring‐closing metathesis reaction, these N‐allyl N‐aryl 2‐alkenamides were respectively converted into corresponding N‐aryl α,β‐unsaturated γ‐lactams in moderate yields.     

H‐transfer reaction during decomposition of N‐(2‐methylpropyl)‐ N‐(1‐diethylphosphono‐2,2‐dimethylpropyl)‐N‐oxyl (SG1)‐based alkoxyamines

Thermal decomposition of four tertiary N‐(2‐methylpropyl)‐N‐(1‐diethylphosphono‐2,2‐dimethylpropyl)‐N‐oxyl (SG1)‐based alkoxyamines (SG1‐C(Me)₂‐C(O)‐OR, R = Me, tBu, Et, H) has been studied at different experimental conditions using ¹H and ³¹P NMR spectroscopies. This experiment represents the initiating step of methyl methacrylate polymerization. It has been shown that H‐transfer reaction occurs during the decomposition of three alkoxyamines in highly degassed solution, whereas no products of H‐transfer are detected during decomposition of SG1‐MAMA alkoxyamine. The value of the rate constant of H‐transfer for alkoxyamines 1 (SG1‐C(Me)₂‐C(O)‐OMe) and 2 ( SG1‐C(Me)₂‐C(O)‐OtBu) has been estimated as 1.7 × 10³ M^?1s^?1. The high influence of oxygen on decomposition mechanism is found. In particular, in poorly degassed solutions, nearly quantitative formation of oxidation product has been observed, whereas at residual pressure of 10^?5 mbar, the main products originate from H‐atom transfer reaction. The acidity of the reaction medium affects the decomposition mechanism suppressing the H‐atom transfer. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013     

2‐Benzothiazolyl‐N‐(arenesulfonyl)‐sulfinimidoyl fluorides

2‐Benzothiazolyl‐N‐(arenesulfonyl)‐sulfinimidoyl fluorides were synthesized by the treatment of benzothiazolyl‐2‐sulfur trifluoride with sulfonamides. The reaction of 2‐benzothiazolyl‐N‐ (p‐toluenesulfonyl)‐sulfinimidoyl fluoride with tert‐ butylamine and morpholine gave 2‐benzothiazolyl‐ N‐(arenesulfonyl)‐sulfinimidoyl amides. The reaction of 2‐benzothiazolyl‐N‐(p‐toluenesulfonyl)‐sulfinimi‐ doyl fluoride or 2‐benzothiazolyl‐¹⁵N‐(p‐tosyl)sul‐ finimidoyl fluoride with S‐trimethylsilylbenzenethiol gave di(benzothiazolyl‐2) disulfide, fluorotrimethylsi‐ lane and N,N′‐bis(p‐toluenesulfonyl)‐N,N′‐bis(phenyl‐ thio)‐hydrazine or ¹⁵N,¹⁵N′‐bis(p‐toluenesulfonyl)‐¹⁵N, ¹⁵N′‐bis(phenylthio)‐hydrazine, respectively. © 2005 Wiley Periodicals, Inc. Heteroatom Chem 16:352–356, 2005; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20102     

Polymorphism of (Z)‐4‐bromo‐N‐(pent‐2‐enyl)‐N‐(3‐phenyl­prop‐2‐ynyl)benzene­sulfonamide

The title compound, C₂₀H₂₀BrNO₂S, has two polymorphic crystal structures with very similar lattice constants. A number of crystals are composites of the two polymorphs. Both crystal structures contain identical layers of mol­ecules. The packing of the layers, however, is different for the two polymorphs.     

N,N′‐Bis(2‐hydroxycyclohexyl)‐N,N′‐bis(2‐hydroxyethyl)ethane‐1,2‐diaminium dichloride

The achiral meso form of the title compound, C₁₈H₃₈N₂O₄²⁺·2Cl⁻, crystallizes to form undulating layers consisting of chains linked via weak hydroxyalkyl C—H...Cl contacts. The chains are characterized by centrosymmetric hydrogen‐bonded dimers generated via N—H...Cl and hydroxycycloalkyl O—H...Cl interactions. trans‐N‐Alkyl bridges subdivide the chains into hydrophilic segments flanked by hydrophobic cycloalkyl stacks along [001].     

Five N′‐benzylidene‐N‐methylpyrazine‐2‐carbohydrazides

The compounds N′‐benzylidene‐N‐methylpyrazine‐2‐carbohydrazide, C₁₃H₁₂N₄O, (IIa), N′‐(2‐methoxybenzylidene)‐N‐methylpyrazine‐2‐carbohydrazide, C₁₄H₁₄N₄O₂, (IIb), N′‐(4‐cyanobenzylidene)‐N‐methylpyrazine‐2‐carbohydrazide dihydrate, C₁₄H₁₁N₅O·2H₂O, (IIc), N‐methyl‐N′‐(2‐nitrobenzylidene)pyrazine‐2‐carbohydrazide, C₁₃H₁₁N₅O₃, (IId), and N‐methyl‐N′‐(4‐nitrobenzylidene)pyrazine‐2‐carbohydrazide, C₁₃H₁₁N₅O₃, (IIe), have dihedral angles between the pyrazine rings and the benzene rings in the range 55–78°. These methylated pyrazine‐2‐carbohydrazides have supramolecular structures which are formed by weak C—H...O/N hydrogen bonds, with the exception of (IIc) which is hydrated. There are π–π stacking interactions in all five compounds. Three of these structures are compared with their nonmethylated counterparts, which have dihedral angles between the pyrazine rings and the benzene rings in the range 0–6°.     

N‐(2‐Bromoethyl)‐4‐piperidino‐1,8‐naphthalimide and N‐(3‐bromopropyl)‐4‐piperidino‐1,8‐naphthalimide

N‐(2‐Bromoethyl)‐4‐piperidino‐1,8‐naphthalimide, C₁₉H₁₉BrN₂O₂, (I), and N‐(3‐bromopropyl)‐4‐piperidino‐1,8‐naphthalimide, C₂₀H₂₁BrN₂O₂, (II), are an homologous pair of 1,8‐naphthalimide derivatives. The naphthalimide units are planar and each piperidine substituent adopts a chair conformation. This study emphasizes the importance of π‐stacking interactions, often augmented by other contacts, in determining the crystal structures of 1,8‐naphthalimide derivatives.     

Strychninium N‐phthaloyl‐β‐alaninate N‐phthaloyl‐β‐alanine and brucinium N‐phthaloyl‐β‐alaninate 5.67‐hydrate

Comparison of the structures of strychninium N‐phthaloyl‐β‐alaninate N‐phthaloyl‐β‐alanine, C₂₁H₂₃N₂O₂⁺·C₁₁H₈NO₄⁻·C₁₁H₉NO₄, and brucinium N‐phthaloyl‐β‐alaninate 5.67‐hydrate, C₂₃H₂₇N₂O₄⁺·C₁₁H₈NO₄⁻·5.67H₂O, reveals that, unlike strychninium cations, brucinium cations display a tendency to produce stacking inter­actions with cocrystallizing guests.     

An interesting cyclization of N‐methyl‐3‐phenyl‐N‐(2‐(Z)‐phenylethenyl)‐cis‐oxiranecarboxamide

Under Lewis acid condition, N‐methyl‐3‐phenyl‐N‐(2‐(Z)‐phenylethenyl)‐cis‐oxiranecarboxamide undergoes elegant double cyclizations to give interesting products.     

(1R,2S)‐2‐[N‐Methyl‐N‐(4‐toluene­sulfonyl)amino]‐1‐phenylpropan‐1‐ol

In the title compound, C₁₇H₂₁NO₃S, the S atom is in a distorted tetrahedral geometry and the N atom exhibits sp² character. The antiperiplanar conformation is observed for the N and hydroxyl‐O atoms and the torsion angle around the N—C linkage is ?136.3 (2)°. The mol­ecules are linked by O—H?O intermolecular hydrogen bonds to form an infinite one‐dimensional chains along the c axis.     

N‐(Ferrocenecarbonyl)‐N′‐(quinolin‐8‐yl)thio­urea

In the title compound, [Fe(C₅H₅)(C₁₆H₁₂N₃OS)], the 8‐am­inoquinoline and acyl­thio­urea moieties are almost planar. There are two perpendicular arrangements of the mol­ecules in the crystal with slightly different conformations. The two cyclo­penta­dienyl rings in each mol­ecule are parallel and eclipsed.     

N-(4-甲基苯甲酰氨基) N’-[5-(2-三氟甲基苯基)-2-呋喃甲酰硫脲的合成、晶体结构测定与生物活性测定

本文首次合成标题化合物N-(4-甲基苯甲酰氨基)-N’-[5-(2-三氟甲基苯基)-2-呋喃甲酰硫脲。化合物(C21H16F3N3O3S, Mr = 447.43)单晶经测定为单斜晶体,空间群为P -1。在晶体中,存在一些分子内和分子间的相互作用,分子间还有C—H···π 的相互作用,这可能导致晶体更稳定的原因。目标产物的结构经IR, H NMR和元素分析测定确证。初步生物活性测试表明,部分化合物对棉花枯萎病、黄瓜灰霉病、苹果轮纹病和棉花炭疽病有较好的选择性杀菌活性;部分目标化合物有较好的除草活性。