Synthesis of tris(aminomethyl)phosphine oxide and its carbon dioxide adduct from tetrakis(hydroxymethyl)phosphonium salts via their methyl carbamate derivatives

1981 ◽  
Vol 59 (1) ◽  
pp. 27-33 ◽  
Author(s):  
Arlen W. Frank
Keyword(s):  
Carbon Dioxide ◽  
Ion Exchange ◽  
Phosphine Oxide ◽  
Convenient Method ◽  
Phosphonium Salts ◽  
Preparative Scale ◽  
C Nmr

Tris(aminomethyl)phosphine oxide (6) can be synthesized from octakis(hydroxymethyl)diphosphonium sulfate (1b) in an overall yield of 54.6% via the methyl carbamate derivatives 2b, 3, and 4. On a preparative scale, the last step is complicated by the formation of a cyclic by-product 8 in amounts up to 20% of the total. The triamine 6 forms a 1:1 adduct (11) with carbon dioxide, whose structure, established by 1H and 13C nmr, consists of equimolar amounts of carbamate A and dicarbamate BC. The components A, B, and C can be separated by ion exchange. Thermolysis of 11 regenerates 6 smoothly, providing a convenient method for purifying the triamine.

The absorption of carbon dioxide by weak base ion exchange resins

AIChE Journal ◽  
1970 ◽  
Vol 16 (4) ◽  
pp. 609-614 ◽  
Author(s):  
Oscar W. Weber ◽  
Irving F. Miller ◽  
Harry P. Gregor
Keyword(s):  
Carbon Dioxide ◽  
Ion Exchange ◽  
Ion Exchange Resins ◽  
Weak Base ◽  
Exchange Resins

Orthogonal Investigation of Influencing Factors on the Modification of Montmorillonite by THPC in Acid Conditions

2014 ◽  
Vol 936 ◽  
pp. 1017-1021
Author(s):  
Pan Chen ◽  
Jin Cheng Wang
Keyword(s):  
Reaction Time ◽  
Ion Exchange ◽  
Influencing Factors ◽  
Reaction Temperature ◽  
Orthogonal Test ◽  
Test Results ◽  
Phosphonium Salts ◽  
Exchange Reactions ◽  
Quaternary Phosphonium Salts

Na-MMT was modified with quaternary phosphonium salts, tetramethylolphosphonium chloride (THPC), via ion-exchange reactions, in acid conditions. Different factors such as reaction time , reaction temperature, the types of solvent, and CEC ratios, were investigated using orthogonal test. Results showed that the best combination of these four factors were A1B3C1D1, that is, the type of the solvent was acetone and water (1:1), reaction time was 3h, CEC ratio was 1:1, and the reaction temperature was 80°C.

scholarly journals On the Formation of COS from H2S and CO2 in the Presence of Zeolite/Salt Compounds

1998 ◽  
Vol 16 (7) ◽  
pp. 577-581 ◽  
Author(s):  
Wolfgang Lutz ◽  
Andreas Seidel ◽  
Bruno Boddenberg
Keyword(s):  
Carbon Dioxide ◽  
Ion Exchange ◽  
Hydrogen Sulphide ◽  
Calcium Ions ◽  
Gaseous Mixture ◽  
Degree Of Conversion ◽  
Low Level ◽  
Sodium Cations

A gaseous mixture of hydrogen sulphide and carbon dioxide (20% H2S, 80% CO2) was brought into contact at 25°C with NaY and NaX zeolites in an as-synthesized form as well as after modification by the inclusion of salts (NaCl, NaBr) in the small cages of the aluminosilicate framework and ion exchange with aqueous CaCl2 solution. At small contact times (5 h), the degree of conversion of H2S according to the reaction H2S + CO2 → COS + H2O by the various samples was found to follow the sequence NaY/NaCl ≈ NaY/NaBr ≈ NaX/NaCl(CaCl2) < NaY « NaX/NaCl ≈ NaX. Long-term runs with NaY and NaY/NaBr revealed that the latter zeolite retained a very low level of H2S conversion for contact times as long as 250 h. It is concluded that such low H2S conversion requires the absence of low-coordinated sodium cations in the supercages or their replacement by calcium ions, and blocking of the β-cages with salt anions.

Etude en rmn 13C de bicyclo[4,n,0]alcanones-3 trans α-substitués. Influence de la nature et de l'orientation du substituant sur le déplacement chimique du 13C du carbonyle

1980 ◽  
Vol 58 (15) ◽  
pp. 1503-1511 ◽  
Author(s):  
Pierre Metzger ◽  
Eliette Casadevall ◽  
André Casadevall ◽  
Marie-José Pouet
Keyword(s):  
Convenient Method ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Uv Spectroscopy ◽  
Substituent Effects ◽  
Fixed Ring ◽  
C Nmr ◽  
Ir And Uv Spectroscopy

The 13C nmr spectra of α, αα, and αα′ substituted trans-fused bicyclo [4,n,0]alkan-3 ones, are described. Substituent effects are discussed in terms of their electron withdrawing character, axial or equatorial configuration, and cyclohexane deformation. 13C=O chemical shifts are shown to be based on the polarization of π bond and on C=O/X non-bonded interactions. As in ir and uv spectroscopy, 13C nmr is a convenient method for detecting an a substituent configuration in fixed ring ketones.

scholarly journals Synthesis and Antimicrobial Screening of Novel 4-Substituted Phenyl-5-[1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl]-2H-1,2,4-triazole-3-thiones

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Namratha Bhandari ◽  
Santosh L. Gaonkar
Keyword(s):  
Convenient Method ◽  
Nmr Spectra ◽  
Spectral Studies ◽  
Antimicrobial Screening ◽  
Antifungal Activities ◽  
H Nmr ◽  
Antibacterial And Antifungal Activities ◽  
Elemental Analyses ◽  
Antibacterial And Antifungal ◽  
C Nmr

The paper describes a convenient method for the preparation of 4-substituted phenyl-5-[1-(4-fluorophenyl)-1,3-dihydroisobenzofuran-5-yl]-2H-1,2,4-triazole-3-thiones. The structures of the synthesized compounds are established by the results of LCMS, 1H NMR, 13C NMR, and IR and elemental analyses. The mercaptotriazoles are indicated to be in thione form by 1H NMR spectra. All the synthesized compounds have been screened for antibacterial and antifungal activities. Compounds 12d and 12h exhibit encouraging results, while the remaining compounds show moderate activities. On the basis of spectral studies, formation of 2-amino-1,3,4-thiadiazoles from the isobenzofuran acyl thiosemicarbazides 11(a–h) is ruled out.

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