Acetone/benzene mixtures

B. a-Ketoglularic acid. The ester obtained by the foregoing procedure is mixed with 600 ml. of concentrated hydrochloric acid and left overnight. The mixture is concentrated by distillation (Note 5) until the temperature of the liquid reaches 140°. It is poured into an evaporating dish and allowed to cool. The solid mass, weighing 11(3-112 g., is then pulverized. The yield of a-ketoglutaric acid is 92-93% of the theoretical for the last step, or 75-77% based upon diethyl succinate. The light tan product, obtained as described above, is suitable for most purposes, but a purer add, m.p. 109-110° (corr.) may be obtained by recrystallization from an acetone-benzene mixture. 

The shift from homogeneous to heterogeneous copolymerization was also noted in acetone-benzene mixtures. The rate was slow, and the system was homogeneous when a benzene (50)-acetone (50) mixed solvent (S = 9.6) was used, but rapid heterogeneous copolymerization was observed in a benzene (80)-acetone (20) mixed solvent (S = 9.3). 

A methyl iodide derivative can be prepared by treating 1.5 g of dimethyl-(pentafluorophenyl)phosphine with 2.0 g of CH3I in 25 ml of absolute ethanol at reflux temperature for 4 hr. On cooling the mixture to room temperature, hygroscopic needles are obtained these are recrystallized from an acetone-benzene mixture to give 1.0 g of colorless needles. The H nmr spectrum of the methyl iodide derivative is a doublet of triplets that is centered at t7.16 with /pH = 14.8 Hz and /ph =1.7 Hz. 

Clathrochelate (HAm)2[FeD3(SnCl3)2] complexes were also formed by cross-linking of the initial nonmacrocyclic iron(II) tris-dioximates with tin(IV) tetrachloride either in acetone or in an acetone-benzene mixture with subsequent addition of amine [71] ... 

Nagata, I. Excess molar enthalpies for methanol + acetone and methanol + acetone + benzene mixtures at 298.15 K Thermochim. Acta 1994,236, 23-30... 

Acetamide [60-35-5] M 59.1, m 81 , pK -1.4, pKl +0.37. Crystd by soln in hot MeOH (0.8mL7g), diltd with Et20 and allowed to stand [Wagner J Chem Educ 7 1135 1930]. Alternate cry sms are from acetone, benzene, chloroform, dioxane, methyl acetate or from benzene-ethyl acetate mixture (3 1 and 1 1). It has also been recrystd from hot water after treating with HCl-washed activated charcoal (which had been... 

Tetra-n-amyiammonium bromide [866-97-7] M 378.5, m 100-101 . Crystd from pet ether, benzene or acetone/ether mixtures and dried in vacuum at 40-50° for 2 days. 

Twenty grams of the resulting oily substances were mixed with 20 grams of silicic acid (Mal-linckrodt Chemical Co.),applied to a column 40 cm in length and 4.5 cm in diameter filled with silicic acid,and eluted with a be nzene-ecetone-methanol mixture. The initial eluate which eluted with a 1 1 0 mixture was discarded and the active fractions eluted with 1 3 0 and 1 3 0.3 mixtures were collected and concentrated to dryness in vacuo. 11 g of this crude substance was then dissolved in a small amount of ethyl acetate and applied to the same silicic acid column as above. After discarding the initial eluates by the 1 1 and 2 1 benzene-acetone mixtures, aclacinomycin 8 fractions were first eluted with the above mixtures of 1 3 and 1 5 ratio, and aclacinomycin A fractions were then eluted with the 1 5 0.5 and 1 5 1 benzene-acetone-methanol mixtures. The eluates were dried over anhydrous sodium sulfate and concentrated to dryness in vacuo. 4,8 g of crude aclacinomycin A and 3.5 g of aclacinomycin 8 were obtained as yellow powder. 

The third double bond can be introduced into the oxepin system by the dehalogenation of appropriate bromine adducts of benzene oxides. 1-Substituted or 3-substituted 2,5-dibromo-7-oxabicyclo[4.1.0]hept-3-enes are converted with sodium iodide in acetone to mixtures of the respective oxepin 1 and benzene oxide 2.12150-156... 

Popova and colleagues47 carried out TLC of oxidation products of 4,4 -dinitrodiphenyl sulphide (the sulphoxide and sulphone) on silica gel + a fluorescent indicator, using hexane-acetone-benzene-methanol(60 36 10 l) as solvent mixture. Morris130 performed GLC and TLC of dimethyl sulphoxide. For the latter, he applied a 6% solution of the sample in methanol to silica gel and developed with methanol-ammonia solution(200 3), visualizing with 2% aqueous Co11 thiocyanate-methanol(2 1). HPLC separations of chiral mixtures of sulphoxides have been carried out. Thus Pirkle and coworkers131-132 reported separations of alkyl 2,4-dinitrophenyl sulphoxides and some others on a silica-gel (Porosil)-bonded chiral fluoroalcoholic stationary phase, with the structure ... 

Figure 12.21 Distillation sequence for the separation of an acetone-heptane mixture using benzene as entrainer.

A mixture of 9.5 g pyrrolyl-2-aldehyde, 29.2 g dimethyl-succinate and NaH (9.6 g of 50% suspension in oil) in 100 ml benzene is stirred at room temperature 6 hours, cooled and carefully acidified with glacial acetic acid. Add water and ether and dry, evaporate in vacuum or work up (JACS 72,501 (1950), JCS 1025(1959)) to get ca. 17 g (80%) 3-methoxycarbonyl-4-(2 -pyrrolyl)-3-butenoic acid (I) (recrystallize-acetone-benzene). A mixture of 12 g (I), 7 g sodium acetate and 70 ml acetic anhydride is left overnight at room temperature with occasional shaking. Then gradually raise the temperature to 70-75° over 2 hours, maintain for 4 hours and work up (see JCS 1714(1955), 986( 1958)) to get ca. 8 g (60%) methyl-4-acetoxy-indole-6-carboxylate (II) (recrystallize-petroleum ether). If desired, this can be converted to 4-OH-indole-6-COOH and 4-methoxyindole-COOH as described in the ref. or decarboxylated as described elsewhere here. If the 1-methyl cpd. is used, 1-Me-indole results. 

For the two insecticides, the soil was extracted with 75, 50 and 50 mL of an acetone benzene methanol (1 2 1 by vol.) mixture. The sample bottles were capped and agitated for 60 minutes on a wrist-action shaker for each extraction. The contents of the bot-... 

Bioventing technology is applicable to contaminants in the vadose zone as well as contaminated regions just below the water table. It is applicable for any contaminant that degrades more readily aerobically than anaerobically. Most applications have targeted the less volatile petroleum hydrocarbons, although the technology has also remediated mixtures that include acetone, benzene, toluene, biphenyl, phenol, methylphenol, naphthalene, and polycyclic aromatic... 

The dimer-rich fractions were adsorbed on 30 parts of Woelm alumina, activity grade IV (i.e., alumina containing 10% water) and eluted first with mixtures of chloroform and cyclohexane and on a second pass with benzene and cyclohexane. Occasionally, acetone-cyclohexane mixtures were used for better separation of alcohols and dimers and nylon powder chromatography for ultimate purification. Even at a 30 1 (alumina lignin) weight... 

Unlike the alternating copolymer, these high yield benzene-insoluble products were not completely soluble in acetone, but they were soluble in a mixture of acetone-benzene (2 1). However, unlike polystyrene, they were precipitated essentially completely when excess benzene was added to the acetone-benzene solutions. In contrast when excess benzene was added to a mixture of polystyrene and the alternating copolymer in an acetone-benzene solution, the copolymer precipitated and the polystyrene remained in the benzene-rich solvent. The polystyrene was recovered from this solution by adding excess methanol. 

Nonmetals. Mixtures of powdered Ni with sulfur or selenium incandesce on heating.11 Organic Solvents. Raney Ni recovered from methanol, ethanol, pentanol, acetone, benzene, cyclohexane, or/vdioxane explodes when heated above 200°C.10 Peroxyformic Acid. Violent explosion with 90% acid.12 Sulfur Compounds. Raney Ni containing the sulfide is pyrophoric.13... 

Mixtures of small molecules (acetone-benzene, ethanol-water) were considered first. In Figures 1 and 2, a comparison is made between the predicted and experimental low-pressure VLE data (21,22) for these systems. An excellent fit to the data is obtained in both cases, with the use of one apparently temperature independent parameter (k j) per binary. 

---