Quinones and quinone methides. IX. Oxidation of 2,4-Bis(1,1-dimethylethyl)-6-(4-methoxyphenylmethyl)phenol in alcoholic solvents: Monomeric products and the crystal structure of an unusual dimes, 2-[3,5-Bis(1,1-dimethylethyl)-2-{methoxy-(4-methoxyphenyl)methoxy} phenoxyl-1,5-bis(1,1-dimethylethyl)-3-[methoxy-(4-methoxyphenyl)methyl]benzene

1981 ◽  
Vol 34 (8) ◽  
pp. 1645 ◽  
Author(s):  
L Jurd ◽  
RY Wong
Keyword(s):  
Crystal Structure ◽  
Silver Oxide ◽  
Crystallographic Analysis ◽  
Quinone Methides ◽  
X Ray ◽  
High Yields ◽  
Methyl Benzene

Oxidation of the title benzylphenol (1) with silver oxide in alcoholic media forms benzylic ethers of type (5) in high yields; e.g. oxidation in methanol yields 2,4-bis(1,1-dimethylethyl)-6-[methoxy(4- methoxyphenyl)methyl]phenol(5a) together with an unusual dimer, the structure of which was shown by X-ray crystallographic analysis to be 2-[3,5-bis(1,1-dimethylethyl)-2-{methoxy(4-methoxyphenyl)- methoxy}phenoxy]-1,5-bis(1,1-dimethylethy)-3-[methoxy(4- methoxyphenyl)methyl]benzene (6). The benzylic ethers (5) are convenient intermediates for the syntheses of a variety of compounds related to (1).

Quinones and quinone methides. X. The crystal structure of a dimeric oxidation product from 2,4-Bis(1,1-dimethylethyl)-6-[(4-methoxyphenyl)methyl]phenol

1984 ◽  
Vol 37 (12) ◽  
pp. 2593
Author(s):  
RY Wong ◽  
L Jurd
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Oxidation Product ◽  
Crystallographic Analysis ◽  
Quinone Methides ◽  
X Ray ◽  
A Minor

The molecular structure of a minor oxidation product of the insect sterilant 2,4-bis(1,1-dimethylethyl) 6-[(4-methoxyphenyl)methyl]phenol has been established as (�)-cis-1,3,6,8-tetrakis(1,1-dimethyl-ethyl)-4b,9b-bis(4-methoxyphenyl)-4b,9b-dihydrobenzofuro[3,2-b]benzofuran by means of X-ray crystallographic analysis.

The Meisenheimer rearrangement in heterocyclic synthesis. II. Synthesis and X-ray crystal structure of a tetrahydro-1H-2,3-benzoxazocine and preparation of a hexahydro-2,3-benzoxazonine

1980 ◽  
Vol 33 (6) ◽  
pp. 1323 ◽  
Author(s):  
JB Bremner ◽  
EJ Browne ◽  
PE Davies ◽  
CLWAH Raston
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Acetic Acid ◽  
Crystal And Molecular Structure ◽  
Phosphorus Oxychloride ◽  
Crystallographic Analysis ◽  
Heterocyclic Synthesis ◽  
Reaction Conditions ◽  
X Ray ◽  
Heterocyclic Derivatives

The heterocyclic derivatives, 8,9-dimethoxy-3-methyl-1-phenyl-3,4,5,6- tetrahydro-1H-2,3-benzoxazocine(3a) and 9,10-dimethoxy-3-methyl-1- phenyl-1,3,4,5,6,7-hexahydro-2,3-benzoxazonine (3b),examples of two new ring systems, have been prepared by Meisenheimer rearrangement of the corresponding 2-benzazepine and 2-benzazocine N-oxide derivatives (2a) and (2b). The Bischler-Napieralski-type cyclization reaction was used in the preparation of the tertiary amine precursors of these N-oxides reaction conditions for the cyclization were critical and phosphorus oxychloride in refluxing butanenitrile was found to give the best yields of the seven- or eight-membered cyclic imine intermediates. Reductive cleavage of the benzoxazocine derivative (3a) with zinc in acetic acid followed by N-methylation gave the expected product, [2-{3- (dimethylamino)propyl}-4,5-di-methoxyphenyl]phenylmethanol (12). The crystal and molecular structure of (3a) has been determined by X-ray crystallographic analysis.

A Novel Alkali-Metal Hydrido-tris(pyrazolyl)borate (Tp*) Complex. Isolation and Crystal Structure of [(Me2CO)3(NaTp*)2]

2014 ◽  
Vol 69 (7) ◽  
pp. 793-798
Author(s):  
Laurent Plasseraud ◽  
Hélène Cattey
Keyword(s):  
Crystal Structure ◽  
Alkali Metal ◽  
Sodium Hydroxide ◽  
Title Compound ◽  
Room Temperature ◽  
Crystallographic Analysis ◽  
Monoclinic Space Group ◽  
Large Excess ◽  
X Ray ◽  
Acetone Water

The title compound was isolated from the treatment of Tp*Sn(Cl)2Bu (1) with a large excess of sodium hydroxide in a mixture of acetone-water at room temperature. [(Me2CO)3(NaTp*)2] (2) crystallizes at 4 °C as prismatic colorless crystals, in the monoclinic space group P21/c with Z = 4, a = 12.2837(6), b = 24.3197(12), c = 16.9547(8) Å, β = 110.017(1)°, and V = 4759.0(4) Å3. The X-ray crystallographic analysis revealed a dinuclear unit in which two Tp*Na moieties are held together by three bridging acetone molecules acting as oxygen-based donors.

The Crystal Structure of Dimethyl (1aα,2aα,5β,6aβ-Hexahydroazirino[2,1-b]benzoxazole-1a, 5(1H)-dicarboxylate

1991 ◽  
Vol 44 (8) ◽  
pp. 1145 ◽  
Author(s):  
MF Mackay ◽  
M Campbell ◽  
MJ Mcleish
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Crystallographic Analysis ◽  
Aminobenzoic Acid ◽  
X Ray ◽  
Relative Stereochemistry

The title compound formed the major component in a rearrangement of an analogue of 4-amino-4-deoxychorismic acid (1), an intermediate in the chorismate-p-aminobenzoic acid biotransformation. X-Ray crystallographic analysis has defined the relative stereochemistry at the four chiral centres in the tricyclic molecule.

The direct electrochemical synthesis of thiolato complexes of cobalt and nickel, and the crystal structure of bis(phenylthiolato)bis(1,10-phenanthroline)cobalt(III) perchlorate

1988 ◽  
Vol 66 (9) ◽  
pp. 2151-2156 ◽  
Author(s):  
Raj K. Chadha ◽  
Rajesh Kumar ◽  
Jaime Romero Lopez-Grado ◽  
Dennis G. Tuck
Keyword(s):  
Crystal Structure ◽  
Electrochemical Oxidation ◽  
Electrochemical Synthesis ◽  
Crystallographic Analysis ◽  
High Yield ◽  
X Ray ◽  
Metal Anode ◽  
Aerial Oxidation ◽  
Perchlorate Salt ◽  
Cobalt And Nickel

Cobalt(II) and nickel(II) thiolates, M(SR)2, can be prepared in high yield by the electrochemical oxidation of a metal anode in an acetonitrile or acetone solution of RSH (R = C6H5, o-CH3C6H4, 2-C10H7, 2,3,4,5-C6F4H; not all combinations). When 2,2-bipyridine or 1,10-phenanthroline (=L) is added to the electrolyte phase, the products are the adducts M(SR)2L2. In the case of Co(SC6H5)2(phen)2, aerial oxidation leads to the formation of the cobalt(III) cation [Co(SC6H5)2(phen)2]+, isolated as the perchlorate salt. X-ray crystallographic analysis showed that this cation has a cis-CoS2(N2)2 kernel.

CRYSTAL STRUCTURE AND X-RAY CRYSTALLOGRAPHIC ANALYSIS OF THE BINUCLEAR CLUSTER THIOCYANATE COMPLEX OF NIOBIUM(IV)

2021 ◽  
Vol 62 (10) ◽  
pp. 1531-1542
Author(s):  
A. D. Fedorenko ◽  
I. S. Fomenko ◽  
M. I. Gongola ◽  
N. V. Pervukhina ◽  
A. V. Kalinkin ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Crystallographic Analysis ◽  
Thiocyanate Complex ◽  
X Ray ◽  
Binuclear Cluster

Darstellung und Kristallstrukturbestimmung von 1,2-Di-t-butyl-1,2-diiodo- diarsan (t-C4H9AsI)2 und Synthese von 1,2,3,4-Tetrakis(t-butyl)tetraarsetan (t-C4H9As)4 über selektive Reduktion von t-Butylarsendiiodid t-C4H9AsI2 Synthesis and Crystal Structure of 1,2-Di-t-butyl-1,2-diiododiarsane (t-C4H9AsI)2 and Synthesis of 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4 via Selective Reduction of t-Butylarsenic Diiodide t-C4H9AsI2

1997 ◽  
Vol 52 (7) ◽  
pp. 790-794 ◽  
Author(s):  
Klaus Megges ◽  
Evgeni V. Avtomonov ◽  
Jörg Lorberth
Keyword(s):  
Crystal Structure ◽  
Low Temperatures ◽  
Selective Reduction ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Elemental Analyses ◽  
High Yields ◽  
C Nmr

Abstract 1,2,3,4-Tetrakis(t-butyl)tetraarsetane (t-C4H9As)4(4) has been synthesized by reduction of t-butylarsenic (III) diiodide (1) with equivalent quantities of either Mg, Ca, Zn, Li, or CoCp2 in THF at low temperatures in high yields. Treatment of 1 with CoCp2 in a molar ratio 1:1 in n-pentane at -78 °C leads to the formation of 1,2-di-t-butyl-1,2-diiododiarsine (2) (t-C4H9AsI)2 in 69 % yield. The products have been characterized by spectroscopic methods (H, 13C-NMR, EI-MS) and elemental analyses. The crystal structure of 2 has been determined by X-ray diffraction methods.

scholarly journals Synthetic Studies on Potent Marine Drugs: Synthesis and the Crystal Structure of 6-tert-butyl-4-phenyl-4H-chromene-2-carboxylic Acid

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Hui-Jing Li ◽  
Jun-Li Wang ◽  
Rui Wang ◽  
Dong-Hui Luo ◽  
Yan-Chao Wu
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Carboxylic Acid ◽  
Methyl Ester ◽  
Crystallographic Analysis ◽  
Antitumor Antibiotic ◽  
Stacking Interactions ◽  
X Ray ◽  
Structural Activity Relationship ◽  
Derivatives Of

4H-Chromene-2-carboxylic acid ester derivatives of renieramycin M might be of use for the structural-activity relationship studies of antitumor antibiotic tetrahydroisoquinoline natural products. Accordingly, 6-tert-butyl-4-phenyl-4H-chromene-2-carboxylic acid, one key intermediate, was synthesized via the condensation of (3E)-2-oxo-4-phenylbut-3-enoate methyl ester with 4-tert-butylphenol in the presence of AuCl3/3AgOTf (5 mol%), followed by cyclodehydration and aqueous hydrolysis. The product was unambiguously shown to the 4H-chromene-2-carboxylic acid by spectroscopy and X-ray crystallographic analysis. A packing diagram of the crystal structure shows that aromaticπ-stacking interactions and O–H⋯O hydrogen bond stabilize the structure in the solid.

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