Hexane-acetone solvent

Summary Hexanitrotetrachloroazobenzene is prepared by reacting 90% nitric acid, 30% fuming sulfuric acid, and 98% sulfuric acid with 3,5-dichloroaniline. The reaction mixture is then heated, and then poured over ice to precipitate the product. The product is then collected by filtration, and then recrystallized from an acetone/hexane solvent mixture to yield pure HNTCAB. Commercial Industrial note For related, or similar information, see Application No. 946,859, December 29, 1986, by Texas Explosives Co. Inc., to David M. O Keefe, Mansfield, TX. Part or parts of this laboratory process may be protected by international, and/or commercial/industrial processes. Before using this process to legally manufacture the mentioned explosive, with intent to sell, consult any protected commercial or industrial processes related to, similar to, or additional to, the process discussed in this procedure. This process may be used to legally prepare the mentioned explosive for laboratory, educational, or research purposes. 

Matrix Spike and Matrix Spike Duplicate Samples— Add 1.0 mL of spiking solution to the sample just after the addition of the surrogate and prior to the addition of the acetone-hexane solvent. 

Many procedures have been studied for detoxification of aflatoxkis, including heat and treatment with ammonia, methylamine, or sodium hydroxide coupled with extraction from an acetone—hexane—water solvent system. Because ki detoxification it is important to free the toxki from cellular constituents to which it is bound, a stabifi2ation of protekis uskig a tanning compound such as acetaldehyde (qv) or glutaraldehyde may be a solution to the problem (98). 

P,17P-Dihydroxyestr-4-en-3-one 1-acetate. The 6-hydroxy compound is removed from the column with 15-17% acetone. Recrystallization of the crude product (1.92 g) from acetone-hexane gives 1.25 g of crystals melting at 165-166° and 0.13 g melting at 162-164° (12.1% yield). When the analytical sample was prepared from the same solvent mixture, the melting point rose to 192-193° (Lit 166° 189-190°) [a] -59.5° (CHCI3) 2, 236 m/i (fi 14,500). 

The mixture is distilled until most of the ether has been removed and then refluxed for 8 hr. Ethyl acetate is added to decompose the excess reagent and concentrated aqueous sodium sulfate is then added until the precipitate begins to adhere to the sides of the flask. Finally ca. 100 g of solid sodium sulfate is added, the salts are removed by filtration and washed well with dioxane. Evaporation of the solvent gives a solid residue which is dissolved in 60 ml of chloroform and shaken with 3.5 g of manganese dioxide for 16 hr. Subsequently another 3.5 g of manganese dioxide is added and shaking continued for a further 16 hr. The solid is removed by filtration and washed well with hot chloroform. Evaporation of solvent and crystallization of the residue from acetone-hexane affords 0.51 g (72%) of 17a-hydroxy-17jff-ethylandrost-4-en-3-one mp 145-148°. 

Irradiations of Testosterone Acetate (114), —In t-Butanol. 1.25 g of (114) in 250 ml t-butanol is irradiated for 32 hr at 30° under nitrogen with a Hanau Q81 high-pressure mercury lamp placed in a central water-cooled Pyrex immersion well with acetone filter. The solvent is evaporated in vacuo and the residue chromatographed on 125 g silica gel with benzene-ethyl acetate (4 1) to yield 0.29 g 17 -hydroxy-la,5 -cyclo-10a-androstan-2-one acetate [(118) 23%] mp 164-165°, after crystallization from acetone-hexane [a]i3 37 (CHCI3) 0.14 g cyclopentanone (120) (11%) mp 106-107° [aJo 38° (CHCI3) and 0.58 g starting material [(114) 46%]. Ratio (118) (120) - 2 1. 

Group D Gasoline, hexane, naphtha, benzene, butane, propane, alcohols, acetone, lacquer, solvent vapors, or natural gas (methane)... 

Azido-2-methylquinoline (4, R - Me 0.500 g, 2.7 mmol) and NaOMc (4.0 g. large excess) in a mixture of MeOH (70 mL) and dioxane (70 mL) was irradiated for 30 min with a 400-W high pressure Hg lamp (Pyrex filter). The solvents were removed in vacuo and ice-water (20 mL) was added. The mixture was extracted with CH2C12 and the extract was washed with H20, dried and evaporated. The residue was chromatographed (silica gel, 1 % acetone/CH2Cl2) to give 5a yield 0.194 g (38%) pale-yellow prisms (acetone/hexanes) mp 78-79 C. 

A mixture of 1.44 g. (0.0099 mole) of indole-3-carboxaldehyde,2 7.0 g. (0.053 mole) of diammonium hydrogen phosphate, 30 g. (30 ml., 0.34 mole) of 1-nitropropane, and 10 ml. of glacial acetic acid is refluxed for 12.5 hours. During the reflux period the pale-yellow mixture becomes dark red. The volatile reactants and solvent are removed under reduced pressure, and an excess of water is then added to the dark residue. After a short time, crude indole-3-carbonitrile precipitates rapidly. It is separated by filtration and dried under reduced pressure weight 1.20-1.34 g. (85-95%). Crystallization from acetone-hexane, with decoloriza-tion by activated carbon, yields 0.68-0.89 g. (48-63%) of fairly pure indole-3-carbonitrile, m.p. 179.5-182.5° (Note 1). 

Transfer the residue with 1 g of Florisil PR on to the top of the column packed with 9 g of Florisil PR with the aid of hexane. Rinse the column with 150 mL of hexane-acetone (4 1, v/v). Elute acetamiprid with 120 mL of a mixed solvent of acetone-hexane (1 1, v/v) and concentrate the eluate to near dryness by rotary evaporation at 40 °C. Dissolve the residue with 5 mL of distilled water and apply the solution to the top of the packed Sep-Pak Ci8 column pretreated with 20 mL each of methanol and distilled water. Elute acetamiprid with 30 mL of a mixed solution of water-acetonitrile (17 3, v/v). Concentrate to dryness on a water-bath at ca 40 °C by rotary evaporation. Prepare the GC-ready sample by dissolving the residue in acetone. 

Sodium sulfate, anhydrous, ACS grade (Fisher Scientific) or equivalent Solvents acetonitrile (ACN), acetone, hexane, methanol (MeOH) and water (pesticide or FIPLC grade)... 

Costley et al. [113] have evaluated the use of a range of organic solvents (dichloromethane, water, acetone, hexane, xylene) in the microwave extraction of oligomers from PET and have compared MAE to alternative extraction approaches (Soxhlet, Pan-bomb). 

PCBs in biological samples are usually extracted by a Soxhlet column and with a nonpolar solvent such as hexane. The sample is first mixed with sodium sulfate to remove moisture. The extraction of PCBs from sediments was tested with sonication, with two sonications interspersed at a 24-h quiescent interval, with steam distillation, or with Soxhlet extraction (Dunnivant and Elzerman 1988). Comparison of the recoveries of various PCB mixtures from dry and wet sediments by the four techniques and the extraction efficiency of four solvents showed that the best overall recoveries were obtained by Soxhlet extraction and the two sonication procedures. In comparisons of solvent systems of acetone, acetonitrile, acetone-hexane (1+1), and water-acetone-isooctane (5+1.5+1), recoveries of lower chlorinated congeners (dichloro- to tetrachloro-) were usually higher with acetonitrile and recoveries of higher chlorinated congeners (tetrachloro- to heptachloro-) extracted with acetone were superior (Dunnivant and Elzerman 1988). The completeness of extraction from a sample matrix does not seem to discriminate against specific isomers however, discrimination in the cleanup and fractionation process may occur and must be tested (Duinker et al. 1988b). 

The mixed solvent ether-acetone-hexane-heptane (2 1.1 1) proved to be an excellent solvent system for the residue analysis of all three compounds with the shaking method. Soxhlet extraction with chloroform, gave quite... 

Many extraction solvents have been used, of which the more polar protic solvents are found to perform best. While Soxhlet recoveries for NPEO are reported at 70% using pentane [13], and 80% using acetone/ hexane [13], solvents like propanol or methanol yield higher recoveries, especially for the higher ethoxylates. 

Two studies compared sonication with Soxhlet extraction with pentane [13], acetone/hexane [13] and hexane/ispropyl alcohol (70 30) [5], The first two Soxhlet extraction solvents yielded lower recoveries than sonication, but the most polar solvent hexane/isopropyl alcohol gave recoveries and relative standard deviations for NP and NPE0i i9 comparable with sonication with hexane/acetone [5],... 

Baker Chemical Co. Molinate sulfoxide was prepared by reacting [ring- Cjmolinate with equimolar m-chloroperbenzoic acid in chloroform (10). The product was puriTied by preparative thin-layer chromatography (TLC) using acetone hexane (1 1) as the developing solvent. The final radiopurity was 98%,... 

Photolytic. Photolysis of permethrin in aqueous solutions containing various solvents (acetone, hexane, and methanol) under UV light (1 >290 nm) or on soil in natural sunlight initially resulted in the isomerization of the cyclopropane moiety and ester cleavage. Photolysis products identified were 3-phenoxybenzyldimethyl acrylate, 3-phenoxybenzaldehyde, 3-phenoxybenzoic acid, mono-chlorovinyl acids, cis- and fra/is-dichlorovinyl acids, benzoic acid, 3-hydroxybenzoic acid, 3-hydroxybenzyl alcohol, benzyl alcohol, benzaldehyde, 3-hydroxybenzaldehyde, and 3-hydroxybenzoic acid (Holmstead et ah, 1978). 

Surprising effects can also be observed when solvent mixtures are used to dissolve a polymer. There are examples where mixtures of two non-solvents act as a solvent vice versa, a mixture of two solvents may behave like a non-solvent. For example, polyacrylonitrile is insoluble in both, nitromethane and water, but it dissolves in a mixture of the two solvents. Similar behavior can be observed for polystyrene/acetone/hexane and poly(vinyl chloride)/acetone/carbon disulfide. Examples of systems where the polymer dissolves in two pure solvents but not in their mixture are polyacrylonitrile/malonodinitrile/dimethylforma-mide and poly(vinyl acetate)/formamide/acetophenone. These peculiarities are especially to be taken into account if one wants to adjust certain solution properties (e.g., for fractionation) by adding one solvent to another. 

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