Semi-preparative LC-SPE-cryoflow NMR for impurity identifications: use of mother liquor as a better source of impurities

2013 ◽  
Vol 51 (9) ◽  
pp. 517-522
Author(s):  
Frank Rinaldi ◽  
Junying Fan ◽  
Charles Pathirana ◽  
Venkatapurim Palaniswamy
Keyword(s):  
1986 ◽  
Vol 51 (11) ◽  
pp. 2481-2488
Author(s):  
Benitto Mayrhofer ◽  
Jana Mayrhoferová ◽  
Lubomír Neužil ◽  
Jaroslav Nývlt

The paper presents a simple model of recrystallization with countercurrent flows of the solution and the crystals being purified. The model assumes steady-state operating conditions, an equilibrium between the outlet streams of each stage, and the same equilibrium temperature and distribution coefficient for all stages. With these assumptions, the model provides the basis for analyzing the variation in the degree of purity as a function of the number of recrystallization stages. The analysis is facilitated by the use of a diagram constructed for the limiting case of perfect removal of the mother liquor from the crystals between the stages.


1987 ◽  
Vol 40 (1) ◽  
pp. 1-6 ◽  
Author(s):  
ISAAC O. KIBWAGE ◽  
GERARD JANSSEN ◽  
ROGER BUSSON ◽  
Jos HOOGMARTENS ◽  
HUBERT VANDERHAEGHE ◽  
...  
Keyword(s):  

2021 ◽  
pp. 105102
Author(s):  
Arthur Merkel ◽  
Matej Vavro ◽  
Martin Ondrušek ◽  
Daria Voropaeva ◽  
Andrey Yaroslavtsev ◽  
...  
Keyword(s):  

2021 ◽  
Vol 5 (1) ◽  
pp. 5
Author(s):  
Evgeny V. Nazarchuk ◽  
Dmitri O. Charkin ◽  
Oleg I. Siidra

Three new uranyl sulfates, [pyH](H3O)[(UO2)3(SO4)4(H2O)2] (1), [pyH]2[(UO2)6(SO4)7(H2O)] (2), and [pyH]2[(UO2)2(SO4)3] (3), were produced upon hydrothermal treatment and successive isothermal evaporation. 1 is monoclinic, P21/c, a = 14.3640(13), b = 10.0910(9), c = 18.8690(17) Å, β = 107.795(2), V = 2604.2(4) Å3, R1 = 0.038; 2 is orthorhombic, C2221, a = 10.1992(8), b = 18.5215(14), c = 22.7187(17) Å, V = 4291.7(6) Å3, R1 = 0.030; 3 is orthorhombic, Pccn, a = 9.7998(8), b = 10.0768(8), c = 20.947(2) Å, V = 2068.5(3) Å3, R1 = 0.055. In the structures of 1 and 2, the uranium polyhedra and SO4 tetrahedra share vertices to form ∞3[(UO2)3(SO4)4(H2O)2]2− and ∞3[(UO2)6(SO4)7(H2O)]2− frameworks featuring channels (12.2 × 6.7 Å in 1 and 12.9 × 6.5 Å in 2), which are occupied by pyridinium cations. The structure of 3 is comprised of ∞2[(UO2)2(SO4)3]2− layers linked by hydrogen bonds donated by pyridinium cations. The compounds 1–3 are formed during recrystallization processes, in which the evaporation of mother liquor leads to a stepwise loss of hydration water.


2010 ◽  
Vol 71 (3-4) ◽  
pp. 225-231 ◽  
Author(s):  
Xinrong Dong ◽  
Yizeng Liang ◽  
Bing Wang ◽  
Xiaohong Long

2005 ◽  
Vol 43 (1) ◽  
pp. 71-76 ◽  
Author(s):  
Hideo Miki ◽  
Tomonobu Terashima ◽  
Yusuke Asakuma ◽  
Kouji Maeda ◽  
Keisuke Fukui
Keyword(s):  

2019 ◽  
Vol 42 (1) ◽  
pp. 19-22
Author(s):  
Hong-Wu Xu ◽  
Li-Huan Wu ◽  
Qiang Ren ◽  
Cui-Yu Liu ◽  
Guan-Qing Yan

Abstract We report here the coordination-mediated resolution of methyl o-chloromandelate, which is a key intermediate for clopidogrel, in preparative scale. The reaction of CaO, optically pure (2R, 3R)-O,O′-dibenzoyltartaric acid, and methyl o-chloromandelate in ethanol solution afforded a mixed-ligands calcium(II) complex that was further purified by stirring of the crystals in hot methanol. Methyl (R)-o-chloromandelate was obtained in good enantiomeric excess value (>99.5%) and yield (71%) by treatment of the complex with acid. At the same time, (2R, 3R)-O,O′-dibenzoyltartaric acid was recovered in 72% yield. In addition, methyl (S)-o-chloromandelate was obtained in good enantiomeric excess value (>99.5%) and yield (73%) by recovery from the mother liquor and resolution with the same procedure for methyl (R)-o-chloromandelate, except that (2S, 3S)-O,O′-dibenzoyltartaric acid was used as the resolving reagent.


2018 ◽  
Vol 7 (1.8) ◽  
pp. 185 ◽  
Author(s):  
Yousef Mubarak

Relatively pure and coarse crystalline potassium sulfate of about 52 wt % K2O content and almost chlorine free has been obtained by reacting commercial potassium chloride and commercial ammonium sulfate in a stirred tank reactor at moderately low temperature. To increase the yield of potassium sulfate to a reasonable value, an evaporation stage located between the reactor and the crystallizer is used. The main steps of the production process include dissolution, reaction, evaporation, crystallization, centrifuging, drying, and then cooling. It is found that the best operating parameters to produce potassium sulfate of good quality, quantity, and crystal size are 1:1 as KCl/ (NH4)2SO4 mole ratio, 60 ºC reaction temperature, 1 hour reaction time, about one third of the total water used in the dissolution step is to be evaporated, 10 ºC crystallization temperature, 1 hour crystallization time, and 160 and 60 rpm agitation speeds in the reactor and the crystallizer respectively. Applying these operating conditions, a potassium sulfate yield of about 78 % can be achieved. Also, a fully soluble complex salt as a mixture of ammonium chloride and potassium sulfate is obtained by further treatment of the mother liquor. Further concentration of the mother liquor by further water evaporation of about 40 wt % and then crystallization of the slurry at 25 oC can recover up to about 60 wt % of the remaining solid in the mother liquor as a complex salt. The total yield of potassium sulfate is found to be about 95 wt % and the whole value of the solid product obtained is about 79 wt %.


Sign in / Sign up

Export Citation Format

Share Document