Analysis of Second Mother Liquor

Analysis of First Mother Liquor A613 R Analysis of Second Mother Liquor A615-L Analysis of First Clear Liquor A615-L Analysis of Lime Treatment Tank A615-R Analysis of Second Clear Liquor A616-L Analysis of Crude Sodium Azide Liquor A616-L... 

Floriani has recently examined bark from Aspidosperma quebracho bianco Schlecht f. pendulas Speg, in which he found the known alkaloids, quebrachine (yohimbine) and aspidospermine, as well as Hesse s aspidosamine, C2gH2g02N2, and a new base, aspidospermicine, Ci Hj ON, l-SHjO (1938). Hartmann and Schlittler have shown that the alkaloid vallesine from Vallesia glabra (Apocynaceae) is aspidospermine, and this has been confirmed by Deulofeu et aJ. who have also found it in V. dichotoma. Later Schlittler and Rottenberg by chromatographic analysis of the mother liquors of aspidospermine isolated a second alkaloid for which they used the old name Vallesine (1948). ... 

Acetamido-2-deoxy-D-glucopyranose (4 85 g) was dissolved in water (400 mL) the pH of the solution was adjusted to 11 with 5 M sodium hydroxide and the solntion was left for 1 day at room temperature. The mixture was deionized with Dowex 50-X8 (H+) resin and evaporated to dryness under vacuum. The residue was taken up with ethanol (300 mL) and heated on the steam bath with stirring. On cooling 4 crystallized (66 g) the mother liquor was concentrated, and a second crop of 4 (5 g) was obtained. Concentration of the second mother liquor gave a third crop (3.5 g) of 4. The recovered 4 was re-treated in the same way. Both residual syrups afforded a mixture of 4 and 5 (17.1 g) containing 88% of 5 according to NMR-spectral analysis. 

To 27.5 g. (0.1 mole) of crude (carbonato)bis(ethylenediamine)-cobalt(III) chloride is added 200 ml. of 1.00 N hydrochloric acid. The carbonato complex is dissolved with evolution of carbon dioxide gas and formation of a red solution consisting primarily of the corresponding cw-diaqua species. The solution is evaporated in the steam bath until an almost dry paste has been formed. The purple residue is filtered and washed with three 20-ml. portions of ice-cold water. Drying in air yields 19.5 g. of purple crystals of cu-dichlorobis(ethylenediamine)cobalt(III) chloride. The mother liquor and the washings are again evaporated almost to dryness to yield a second crop of crystals, 5.9 g. The total yield is 25.4 g. (84% based on (carbonato)bis(ethylenediamine)cobalt(III) chloride). The analysis and the visible absorption spectrum of the two fractions are identical. Anal. Calcd. for [Co(en)2Cl2 ] C1 H20 Co, 19.42 N, 18.46 C, 15.82 Cl, 35.05 H, 5.98. Found Co, 19.50 N, 18.57 C, 15.77 C1, 35.15 H, 6.01. 

IX)Lime Treatment Tank contained liquor obtained from the wringer producing the second wringer cake. The liquor normally contained ca 9-10% NaN, 10-13% NaOH and up to 0.75% Na2C03. Its sp gr by hydrometer was ca 1.2. An 8-oz sample was taken,and after analysis according to item VI (First Mother Liquor), the amt of iime necessary to ppt the carbonate as CaCOj was calcd and... 

Further concentrate the mother liquors from the second crop to a volume of 3-4 ml. The resulting oil contains crude 2-bromonitrobenzene. Separate the oil from the two-phase mixture by means of a Pasteur pipet and weigh and reserve it for chromatographic analysis (Parts B and C). 

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