scholarly journals Studies on Steroidal Compounds. XII. Stereochemistry of 1, 4-Addition of Grignard Reagent for α, β-Unsaturated Steroidal Ketones. Grignard Reaction of 3β-Hydroxycholest-4-en-6-one

1964 ◽  
Vol 12 (10) ◽  
pp. 1224-1231 ◽  
Author(s):  
Hiromu Mori
2010 ◽  
Vol 5 (2) ◽  
Author(s):  
Putu Indrayani ◽  
Aliefman Hakim

Abstrak : Sintesis 6-metil-2-hepten-4-ol diawali dengan pembentukan reagen Grignard isobutilmagnesium bromida pada 400C selama 1 jam, dilanjutkan dengan pembentukan garam alkoksi magnesium bromida pada 00C.Hidrolisis terhadap garam alkoksi magnesium bromida dengan larutan NH4Cl jenuh menghasilkan 6-metil-2-hepten-4-ol. Hasil sintesis kemudian diuji sifat fisiko-kimianya meliputi berat jenis, indeks bias serta identifikasi denganSpektrofotometer Inframerah (IR), Kromatografi Gas (GC) dan Kromatografi Gas-Spektrometer Massa (GC-MS). Hasil sintesis menghasilkan cairan beraroma manis segar, berwarna kekuningan, berat jenis 0,81529 g/mL, indeks bias 1,40830, kemurnian 66,07 % dan hasil 46,31 %. Karakter IR senyawa hasil sintesis menunjukkan vibrasi ulur O-H alkohol pada 3361 cm-1, vibrasi ulur C-OH pada 1049,2 cm-1, vibrasi ulur C=C pada 1676 cm-1 dan serapan 2956,7 dan 2920 cm-1 untuk vibrasi ulur C-H dalam CH 3 dan spektra massa dengan m/e 128 yang dicapai pada waktu retensi 6,284 menit. Data-data tersebut mendukung bahwa senyawa hasil sintesis adalah 6-metil-2-hepten-4-ol.Kata kunci : Sintesis, reaksi Grignard dan 6-metil-2-hepten-4-olAbstract : Synthesis of 6-methyl-2-hepten-4-ol was generated with formation of Grignard reagent Isobutylmagnesium bromide carried out at 400C for one hour, then formation of alcoxide salt magnesium bromide carried out at 00C. Alcoxide salt magnesium bromide were hydrolyzed by saturated NH4Cl solution producing 6-methyl-2-hepten-4-ol. Results were examined physically and chemically including density, refraction index, pure percentage and yield percentage were 0,81529 g/mL, 1,40830, 66,07 % and 46,31 % respectively. The IR characters showed stretching vibration of O-H group at 3361 cm-1, stretching vibration C-OH group at 1049,2 cm-1, stretching vibration C=C group at 1676 cm-1 and absorption of C-H in CH3 2956,7 and 2920 cm-1. Identification using GC-MS resulted spectra m/e 128 at time retention 6,284 minutes. The proven data indicated that the resulted compound was 6-methyl-2-hepten-4-ol.Keywords : synthesis, Grignard reaction and 6-methyl-2-hepten-4-ol


1999 ◽  
Vol 600 ◽  
Author(s):  
S. Tanaka ◽  
K. Takeuchi ◽  
M. Asai ◽  
T. Iso ◽  
M. Ueda

AbstractA hyperbranched conjugated polymer containing triphenylamine was prepared by the Grignard reaction of tris(4-bromophenyl)amine 1, via the coupling of N, N-bis(4-bromophenyl)-N-(4-bromomagnesiophenyl)amine 2 with the catalytic amount of Ni(acac)2. Grignard reagent 2 reacted as an AB2-type monomer to give hyperbranched conjugated polymer 3 in a one-step process. Polymer 3 was also obtained via the Pd-catalyzed coupling of N, N-bis(4-bromophenyl)-4-animobenzeneboronic acid 4. Polymer 3 had an average molecular weight of 4.0–6.3×103 and was found to be soluble in organic solvents such as THF and CHC13. A cast film had an anodic peak at 0.95–1.20 V vs. Ag wire. It was dark blue above the oxidation potential and brown-yellow in the neutral state. When polymer 3 was doped with iodine, its conductivity rose to 0.8–3.0 S/cm


1969 ◽  
Vol 47 (17) ◽  
pp. 3085-3088 ◽  
Author(s):  
W. H. Horspool ◽  
R. G. Sutherland ◽  
J. R. Sutton

RMgBr reacts normally with acylferrocenes to give the corresponding alcohols. RMgI gives good yields of the most highly substituted ferrocenyl ethylene. In solutions of moderate acid strength, α-ferrocenyl carbonium ions lose a proton to form the substituted alkene rather than undergo nucleophilic attack by water to give the corresponding alcohol. Since the alcohols are more basic than the alkenes, it is possible to devise a general synthesis of ferrocenyl ethylenes by the reaction of any Grignard reagent with an acylferrocene.


2013 ◽  
Vol 634-638 ◽  
pp. 2044-2048
Author(s):  
Yang Wang ◽  
Qiang Li ◽  
Xian Feng Gong ◽  
Xue Ling Zhao ◽  
Yu Zhang

2-Hydroxy-6-naphthoic acid is an main raw material for the synthesis of polyaromatic ester, it was synthesized from 2-Naphthol by methoxylation, bromization, grignard reaction and demethylation before recrystallization (C2H5OH:H2O=2.8:1 m/m) with an overall yield of 78.5% and content of 99.1%. Furthermore, the results showed that the 6-bromo-2-methoxynaphthalene was prepared using Sn as reducing agent with 96.2% of the yield which is higher than 6-bromo-2-methoxynaphthalene was prepared using solid carbon dioxide and grignard reagent with 23.8% of the yield.


1989 ◽  
Vol 67 (4) ◽  
pp. 708-709 ◽  
Author(s):  
Annie Grouiller ◽  
Hassan Essadiq

Two C-methylated base nucleosides were obtained when 2′-O-tosyl-5′-O-trityluridine was reacted with 30 equivalents of methylmagnesium iodide. Keywords: nucleoside, Grignard reaction, C-methyl pyrimidinone, anhydro derivative, arabinofuranosyl.


2003 ◽  
Vol 771 ◽  
Author(s):  
Amir Fardad ◽  
Wei Liang ◽  
Yadong Zhang ◽  
Bryson Case ◽  
Shibin Jiang ◽  
...  

AbstractFluorinated and photo-imageable precursors are synthesized through a Barbier-Grignard reaction for 1550-nm window. The precursors are used for the sol-gel process of integrated optic components for silica-on-silicon technology. Material compositions and process parameters are optimized to achieve internal absorptions >0.1 dB/cm and propagation losses of about 0.5 dB/cm at 1550 nm. Compact 1×16 Beam splitters are designed and fabricated which exhibit >0.3 dB power uniformity, >0.1 dB PDL and 1.5 dB coupling loss. By hybrid integration of the passive splitters and in-house fiber amplifiers, amplifying splitters are demonstrated at various signal intensities.


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