Solvent removability

Method 2. Place 90 g. of sodium benzenesulphonate (Section IV,29) (previously dried at 130-140° for 3 hours) and 50 g. of powdered phosphorus pentachloride (1) in a 500 ml. round-bottomed flask furnished with a reflux condenser heat the mixture in an oil bath at 170-180° for 12-15 hours. Every 3 hours remove the flask from the oil bath, allow to cool for 15-20 minutes, stopper and shake thoroughly until the mass becomes pasty. At the end of the heating period, allow the reaction mixture to cool. Pour on to 1 kilo of crushed ice. Extract the crude benzenesulphonyl chloride with 150 ml. of carbon tetrachloride and the aqueous layer with 75 ml. of the same solvent. Remove the solvent under atmospheric pressure and proceed as in Method 1. The yield is about 170 g., but depends upon the purity of the original sodium benzenesulphonate. 

This is a way to do this procedure without having to use one of those crazy tube furnaces stuffed with thorium oxide or manganous oxide catalyst [21]. The key here is to use an excess of acetic anhydride. Using even more than the amount specified will insure that the reaction proceeds in the right direction and the bad side reaction formation of dibenzylketone will be minimalized (don t ask). 18g piperonylic acid or 13.6g phenylacetic acid, 50mL acetic anhydride and 50mU pyridine are refluxed for 6 hours and the solvent removed by vacuum distillation. The remaining residue is taken up in benzene or ether, washed with 10% NaOH solution (discard the water layer), and vacuum distilled to get 8g P2P (56%). 

Once the reaction mix has cooled after reflux, 500mL of room temperature dHsO can be added and the whole solution extracted with DCM. The DCM layer is separated and the solvent removed by distillation to give the li-nitropropene as an oil of all things. This oil can then be recrystallized in hot methanol just like the crystalline form was [38]. 

METHOD 2 [89]--1M MDA or benzedrine and 1M benzaldehyde is dissolved in 95% ethanol (Everclear), stirred, the solvent removed by distillation then the oil vacuum distilled to give 95% yellow oil which is a Schiff base intermediate. 1M of this intermediate, plus 1M iodomethane, is sealed in a pipe bomb that s dumped in boiling water for 5 hours giving an orangy-red heavy oil. The oil is taken up in methanol, 1/8 its volume of dH20 is added and the solution refluxed for 30 minutes. Next, an equal volume of water is added and the whole solution boiled openly until no more odor of benzaldehyde is detected (smells like almond extract). The solution is acidified with acetic acid, washed with ether (discard ether), the MDMA or meth freebase liberated with NaOH and extracted with ether to afford a yield of 90% for meth and 65% for MDMA. That s not a bad conversion but what s with having to use benzaldehyde (a List chemical) Strike wonders if another aldehyde can substitute. 

A solution of 0.21 mol of butyllithium in about 140 ml of hexane (note 1) was cooled below -40°C and 90 ml of dry THF ivere run in. Subsequently a cold (< -20 C) solution of 0.25 nol of propyne in 20 ml of dry THF was added with cooling below -20°C and a white precipitate was formed. A solution of 0.10 mol of anhydrous (note 2) lithium bromide in 30 ml of THF was added, followed by 0.20 mol of freshly distilled cyclopentanone or cyclohexanone, all at -30°C. The precipitate had disappeared almost completely after 20 min. The cooling bath was then removed and when the temperature had reached 0°C, the mixture was hydrolyzed by addition of 100 ml of a solution of 20 g of NHi,Cl in water. After shaking and separation of the layers four extractions with diethyl ether were carried out. The extracts were dried over magnesium sulfate and the solvents removed by evaporation in a water--pump vacuum. Careful distillation of the remaining liquids afforded the following... 

The cinnamate ester prepared as above (23.2 g. 79 mmol) was added as a solid slowly to refluxing xylene (500 ml) over a period of 3 h at a rate that prevented accumulation of unreacted azidocinnamate in the solution (monitored by gas evolution through a gas bubbler). The solution was refluxed for an additional 2 h after gas evolution ceased. The reaction mixture was cooled and the solvent removed in vacuo. The residue was recrystallized from methanol to give pure product (20.7 g, 99% yield). 

A solution of 2,3-dimethylindole (145 g, 1 mol) in dry dioxan containing hydroquinone (100 mg) was treated with JV,JV,JV-trimethylbenzylammonium ethoxide (5 ml of a 40% solution in MeOH) and warmed to 35 C. Freshly distilled acrylonitrile (150 ml, 2.5 mol) was added at a rate such that the temperature did not rise above 40°C. The solution was then stirred overnight and diluted with 10% aq. acetic acid (11). The solution was extracted with CH Clj and the extract was washed with water and dried (MgS04). extract was then mixed with silica gel (800 g) and the solvent removed in vacuo. The silica was placed in a Soxhlet extractor and extracted with cyclohexane. The extract deposited the product as colourless needles (125 g, 63% yield). 

I2O5 (400 mg 1.20 mmol) was added to a solution of a cycloalka[b]indole (l.OOmmol) in 80% aqueous THF (25 ml). The mixture was stirred at room temperature and the solvent removed in vacuo. The residue was extracted into EtOAc and the extract washed with water, 5% NaS203, saturated NaHCOj and brine and dried over Na2S04. The solvent was evaporated and the residue purified by silica gel chromatography. 

In many applications in mass spectrometry (MS), the sample to be analyzed is present as a solution in a solvent, such as methanol or acetonitrile, or an aqueous one, as with body fluids. The solution may be an effluent from a liquid chromatography (LC) column. In any case, a solution flows into the front end of a mass spectrometer, but before it can provide a mass spectrum, the bulk of the solvent must be removed without losing the sample (solute). If the solvent is not removed, then its vaporization as it enters the ion source would produce a large increase in pressure and stop the spectrometer from working. At the same time that the solvent is removed, the dissolved sample must be retained so that its mass spectrum can be measured. There are several means of effecting this differentiation between carrier solvent and the solute of interest, and thermospray is just one of them. Plasmaspray is a variant of thermospray in which the basic method of solvent removal is the same, but the number of ions obtained is enhanced (see below). 

Eventually, not only neutral solvent molecules but also ions start to desorb from the surface. With much of the solvent removed, the ions and residual solvent pass through two chambers, each under partial vacuum to remove more solvent. After passing through the two chambers, the ions are passed to the m/z analyzer. 

Fiber cross sections are also deterrnined by the coagulation conditions or, in the case of dry spinning, by the solvent evaporation process. The skin that forms early in the solvent removal process may remain intact as the interior of the filament deflates from solvent removal. Wet spun fibers from organic solvents are often bean shaped, while those from inorganic solvent systems are often round. Dry spun fibers, such as Du Font s Odon, are... 

The heated polymer solution emerges as filaments from the spinneret into a column of warm air. Instantaneous loss of solvent from the surface of the filament causes a soHd skin to form over the stiU-Hquid interior. As the filament is heated by the warm air, more solvent evaporates. More than 80% of the solvent can be removed during a brief residence time of less than 1 s in the hot air column. The air column or cabinet height is 2—8 m, depending on the extent of drying required and the extmsion speed. The air flow may be concurrent or countercurrent to the direction of fiber movement. The fiber properties are contingent on the solvent-removal rate, and precise air flow and temperature control are necessary. 

Concretes and absolutes, both obtained by total extraction of the plant material and not subject to any form of distillation other than solvent removal, are complex mixtures containing many chemical types over wide molecular weight ranges. In some cases, gas chromatographic analysis shows httle volatile material. Yet these products have powerful odors and contribute in important ways to the perfumes in which they are used. 

Tetraacylates are prepared from titanium tetrabromide and excess carboxyUc acid ia an iaert solvent. After solvent removal, the residue is heated to remove hydrogen bromide. 

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