Celite filter aid

Celite Filter Aids for Maximum Clarity atEowest Cost, Internal Pubhcation No. EA-84, CELITE Corp., Lompoc, Calif., 1984. 

To a cooled (0°), stirred suspension of 10.0 g. (0.0395 mole) of aminomalononitrile p-toluenesulfonate2 in 20 ml. of water is added 10.0 g. (0.204 mole) of sodium cyanide in 30 ml. of ice water. One minute (Note 1) after the addition of the sodium cyanide the precipitated product is collected by filtration and washed with 20 ml. of ice water. The solid is immediately dissolved (Note 1) in 30 ml. of boiling isobutyl alcohol, and the solution is stirred with 0.4 g. of Darco activated carbon (Note 2). The mixture is filtered rapidly through 10 g. of Celite filter aid, and the filter cake is washed with 10 ml. of hot isobutyl alcohol. The product that crystallizes on cooling is collected by filtration and washed with 10 ml. of isobutyl alcohol to give 0.95-1.1 g. (22-26%) of white needles, m.p. 181-183° (dec.). 

Prepare 6-methoxy-l-indanone (I) (JCS 1986(1962)) using polyphosphoric acid made by diluting 500 g of the commercial acid with 120 g 85% phosphoric acid. 2.5 g (I) in 176 ml ether and reflux one hour with 0.27 g lithium aluminum hydride. Cool and carefully add water and filter when bubbling stops (can use Celite filter aid). Dry and evaporate in vacuum and store twelve hours at -15° (under N2 if possible) to precipitate the white 6-methoxy-l-indanol (II) (recrystallize-n-hexane). 2.5 g (II) in 73 ml benzene and reflux one-half hour with 0.2 g p-toluenesulfonic acid. Cool, add water and separate the phases. Extract the aqueous phase with ether and combine with benzene phase and dry, evaporate in vacuum to get 5-methoxy-indene (III) (can distill 110-45/10). 1.53 g (III) and 1.39 g N.N-diethyl-aminoethyl-Cl.HCI in benzene (prepare the free base in benzene as described previously). Reflux four hours with 0.42 g sodamide, cool, wash with water and dry, evaporate in vacuum to get the indene analog of 6-methoxy DET as a dark liquid (can crystallize as oxalate). Alternatively, dissolve 2.51 g (III) in ether and treat (under N if possible) with 12 ml 1.6M buty-Li in hexane at 0-10°. After two hours cool to -30° and add 12 ml more of butyl-Li. Add ether suspension of 2.5 g N,N-diethylaminoethyl-CI. HCI over one-half hour and warm to room temperature. Filter, evaporate in vacuum to get the 6-methoxy-DET analog. 

Celite filter aid neutral aluminium oxide borate buffer pH 7... 

The hydrochloric acid solution is added to speed solution of the nickel salts that otherwise lead to emulsions during separation. If no emulsion is encountered after mixing the petroleum ether and water solutions, no hydrochloric acid need be added. Similarly, the filtration through Celite filter aid is intended to remove finely divided nickel metal and other insoluble particles which complicate the washing procedure. If no particles are present, the filtration step should be omitted. 

The diethyl ether layer is separated and dried over anhydrous MgS04 for 1 to 2h. Filtration, using a medium porosity frit and Celite filter aid, followed by solvent removal under reduced pressure gives an orange gum. 

Cleavage of aromatic benzyl ethers.1 In this reaction, the reagent acts as a Lewis acid. Yields are greatly improved if the solvent is completely removed from the slurry. A high surface area is important to this cleavage, and the Chromosorbs and Celite Filter Aid can replace silica. 

The crude product (48.4 grams, 80.9% yield) was recrystallized from an absolute ethanol-ethyl acetate solvent system by suspending the salt in boiling anhydrous ethyl acetate and just enough absolute ethanol was gradually added to effect solution after which the solution was concentrated to about two-thirds of the original volume on the steam bath, charcoal treated, and suction-filtered through Celite filter aid. The white crystals of 2-dimethylaminoethanol p-acetylaminobenzoate obtained, dried at room temperature at a pressure of 0.08 mm Hg for 15 hours, melted at 159.0°-161.5°C. 

The reaction mixture is filtered over a Celite filter aid and the filtrate is concentrated under vacuum. The resulting material is dissolved in CH2CI2, washed with dilute HCI, NaHC03 and concentrated. The residue is chromatographed over silica gel (1.25 kg) with 5% MeOH 1% NH40H CH2CI2. The N-ethyl-N-heptyl-y-oxo-4-[(methylsulfonyl)amino]... 

Celite, filter aid Hi-C orange drink Hi-C grapefruit drink Hi-C apple drink... 

The solution is poured into H20 (1 L) and filtered (Celite filtering aid may be needed). The filtrate is discarded and the residue is rinsed with chloroform until the washings become colorless. The chloroform solution is then washed with water (200 mL), separated, and taken to dryness. The crude product is chromatographed on alumina with CHCl3/MeOH 10 1 as eluent. Yield 0.80-0.88 g of the p-oxo dimer, which can be crystallized from dichloromethane/methanol or converted to the chloride as described above. 

Considerably improved filtration may be accomplished when the fritted-glass filter is covered with a 1-1.5 cm layer of powdered aluminum (or dried Celite filter aid). Before starting the filtration, the whole apparatus is evacuated. Then the reaction mixture is poured into the fritted-glass filter while nitrogen is introduced slowly into the space above the filter. The solids are washed with 15 ml of benzene and the filtrates are combined to give 262 g of clear yellowish solution. The yield with respect to the initial amount of 2-methoxyethanol is 98.1%. Anal. Calcd. for Na[AlH2(0CH2CH20CH3)2] Na, 11.37 Al, 13.35 H, 0.997%. Found Na, 6.04 Al, 6.94 H, 0.537%, Na Al H = 1.02 1 2.07. 

Cleaning Up Since sucrose, yeast, and ethanol are all natural products, all solutions produced in this experiment contain biodegradable material and can be flushed down the drain after dilution with water. The limewater can be disposed of in the same way. The Celite filter aid can be placed in the nonhazardous solid waste container. 

Cleaning Up Filter the pot residue from the steam distillation through a layer of Celite filter aid on a Buchner funnel. Discard the tin salts in the nonhazardous solid waste container. The filtrate, after neutralization with hydrochloric acid, can be flushed down the drain. 

The soluble portion of celite filter aids is extremely low. 

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