Drierite

Another valuable drying agent of general application is anhydrous calcium sulphate, marketed under the name of Drierite. It is rapid in its action, but has only a limited drying capacity because it forms the hydrate 2CaS04,H20 and thus combines with only 6-6 per cent, of its weight of water. The vapour pressure of the system ... 

You see that vacuum adapter stuck to the top of the condenser in fig. 7a Well, a closer look at it in fig. 7b will show that it has some drying agent sandwiched between two cotton balls and the nipple (tee heel) sealed with plastic wrap or foil. The drying agent can be either a commercial product called Drierite or calcium chloride. This attachment is placed on top of a condenser when refluxing solutions that have no water in them and must remain that way during the time they are refluxed. All this is to prevent moisture in the outside air from coming into contact with the cold surface of the of the inside walls of the condenser. This will surely happen and the condensed outside-air water will drip down into the reaction flask and ruin the experiment. This is not so much a... 

Calcined Anhydrite. Soluble anhydrite, or second-settle stucco, has physical properties similar to those of gypsum plaster. It hydrates to the dihydrate rapidly in water. Its outstanding property is its extreme affinity for any moisture, which makes it a very efficient drying agent (see Desiccants). In ambient moisture-laden air, it readily hydrates to hemihydrate. Soluble anhydrite, under the trade name Drierite, is widely used as a desiccant in the laboratory and in iadustry. A small amount is also used as an insecticide carrier. Small amounts of soluble anhydrite are unintentionally produced in most commercial calciners during hemihydrate production. 

Drierite Product Catalog W. A. Hammond Drierite Co., Xenia, Ohio. 

The 213 g. (0.8 mole) of finely powdered silver salt is placed in a 1-1. three-necked flask (Note 3) two necks of the flask are stoppered, and the third is connected to a water pump through a U-tube or flask containing Drierite. The flask is then placed in an oil bath and evacuated to a pressure of about IS mm. The temperature of the oil bath is maintained at 100-110 for 36 hours (Notes 4 and S). 

Calcium sulfate (anhydrous). (Prepared by heating the dihydrate or the hemihydrate in an oven at 235° for 2-3h it can be regenerated.) Available commercially as Drierite. It forms the hemihydrate, 2CaS04.H20, so that its capacity is fairly low (6.6% of its weight of water), and hence is best used on partially dried substances. It is very efficient (being comparable with phosphorus pentoxide and concentrated sulfuric acid). Suitable for most organic compounds. Solvents boiling below 100° can be dried by direct distillation from calcium sulfate. 

N. Y., 3rd edn, 1970]. Acetone was shaken with Drierite (25g/L) for several hours before it was decanted and distd from fresh Drierite (lOg/L) through an efficient column, maintaining atmospheric contact through a Drierite drying tube. The equilibrium water content is about lO M. Anhydrous Mg(C104)2 should not be used as drying agent because of the risk of EXPLOSION with acetone vapour. 

Nitrobenzyl alcohol [619-73-8] M 153.1, m 93 . Crystd from EtOH and sublimed in a vacuum. Purity should be at least 99.5%. Sublimed samples should be stored in the dark over anhydrous CaSOa (Drierite). It the IR contains OH bands then the sample should be resublimed before use. [Mohammed and Kosower J Am Chem Soc 93 2709 1979.]... 

Fractional crystn was more effective than fractional distn from Drierite in purifying nitromethane for conductivity measurements. [Coetzee and Cunningham J Am Chem Soc 87 2529 7965.] Specific conductivities around 5 x 10 ohm em were obtained. 

Piperazine phosphate (H2O) [18534-18-4] M 197.6. Crystd twice from water, air-dried and stored for several days over Drierite. The salt dehydrates slowly if heated at 70 . 

Also purified by dissolving in CHCI3, adding solid K2CO3 and Drierite, filtering and fractionally distilling through an Sin helix packed column. The sulfate has m 205°, and the picrate (from hot H2O) has m 155-156°. [Frank and Meikle J Am Chem Soc 72 4184 1950.]... 

Nitrous oxide [10024-97-2] M 44.0, h -88.5°. Washed with cone alkaline pyrogallol solution, to remove O2, CO2, and NO2, then dried by passage through columns of P2O5 or Drierite, and collected in a dry trap cooled in liquid N2. Further purified by ffeeze-pump-thaw and distn cycles under vacuum [Ryan and Freeman J Phys Chem 81 1455 1977],... 

A detailed procedure for the use of MCPBA recently appeared in Reagents for Organic Synthesis by Fieser and Fieser. The commercially available MCPBA (Aldrich) is 85% pure the contaminant, m-chlorobenzoic acid, can be removed by washing with a phosphate buffer of pH 7.5. The epoxidation is usually performed as follows a solution of 3 -acetoxy-5a-androst-16-ene (2.06 g, 6.53 mmoles) in 25 ml of chloroform (or methylene dichloride) is chilled to 0° in a flask fitted with a condenser and drierite tube and treated with a solution of commercial MCPBA (1.74 g, 20% excess) in 25 ml chloroform precooled to the same temperature. The mixture is stirred and allowed to warm to room temperature. After 23 hr (or until TLC shows reaction is complete) the solution is diluted with 100 ml chloroform and washed in sequence with 100 ml of 10% sodium sulfite or sodium iodide followed by sodium thiosulfate, 200 ml of 1 M sodium bicarbonate and 200 ml water. The chloroform extract is dried (MgS04) and evaporated in vacuo to a volume of ca. 10 ml. Addition of methanol (10 ml) followed by cooling of the mixture to —10° yields 0.8 gof 16a,17a-epoxide mp 109.5-110°. Additional product can be obtained by concentration of the mother liquor (total yield 80-90%). 

The dry tosylhydrazone (20 g, 45.5 mmol) is dissolved in 750 ml of 1,2-dimethoxyethane (freshly distilled from lithium aluminum hydride) in a flame-dried 1 liter round bottom flask fitted with a 240 ml addition funnel, a drierite tube and a magnetic stirrer. A 2.05 M ether solution of methyllithium (130 ml, Alfa Inorganics, Inc.—Caution to avoid the mineral oil impurity the methyllithium solution is decanted from a cold solution which contains a precipitate) is placed in the dropping funnel and added over a 60 min period. The temperature of the reaction mixture increases to ca. 35° during the addition however, no cooling precautions are required. The highly colored reaction mixture is stirred for 7 hr and then poured into 1.5 liters of ice water. The flocculent precipitate is digested for 12 hr at room temperature to speed the filtration. After filtration the filter cake is washed with 500 ml water and dried under vacuum at 50° for several hr. The androsta-5,16-dien-3l5-ol is obtained in ca. 70% yield after recrystallization from methanol mp 138-139°. 

A mixture of the epoxide ca. 5 mmol), sodium azide (6 g, activated by the method of Smith) and 0.25 ml of concentrated sulfuric acid in 70 ml of dimethyl sulfoxide is heated in a flask fitted with a reflux condenser and a drierite tube on a steam bath for 30-40 hr. (Caution carry out reaction in a hood.) The dark reaction mixture is poured into 500 ml of ice water and the product may be filtered, if solid, and washed well with water or extracted with ether and washed with sodium bicarbonate and the water. The crude azido alcohols are usually recrystallized from methanol. 

One important factor to consider in the preparation of the organic phase is the presence of inhibitors in the monomers. Some formulae call for the removal of inhibitors, primarily TCB, from the monomers. The TCB inhibitor forms highly colored complexes with metallic salts rendering the final product colored. Styrene has about 50 ppm of TCB. DVB, being more reactive, contains about 1000 ppm of TCB. There are several options for the removal of inhibitors. Columns packed with DOWEX MSA-1 or DOWEX 11 ion-exchange resins (Dow Chemical Company) can be used. White drierite or activated alumina also works well. 

Calcium sulfate, CaS04> is used as a drying agent and sold under the trade name Drierite. For the reaction... 

Two absorbents are required, one for water vapour, the other for carbon dioxide. The absorbents for water vapour which are generally employed are (a) anhydrous calcium chloride (14-20 mesh), (b) anhydrous calcium sulphate ( Drierite or Anhydrocel ), and (c) anhydrous magnesium perchlorate ( Anhydrone ). Both (b) and (c) are preferable to (a) (c) absorbs about 50 per cent of its weight of water, but is expensive. Anhydrous calcium chloride usually contains a little free lime, which will absorb carbon dioxide also it is essential to saturate the U-tube containing calcium chloride with dry carbon dioxide for several hours and then to displace the carbon dioxide by a current of pure dry air before use. 

A. N-Trijluoroacetanilide. In a two-necked, round-bottomed flask fitted with a thermometer, a Drierite tube, and a magnetic stirring bar are placed 4.56 ml. (4.66 g., 0.050 mole) of aniline [Benzenamine] (Note 1) and 15 ml. of dimethyl sulfoxide (Note 2). The resulting solution is stirred and cooled in an ice water bath, and when the internal temperature has dropped to 10-15°, 21.5 g. (0.10 mole) of 1,1,1-tri-chloro -3,3,3 -trifiuoroacetone [2 -Propanone, 1,1,1 -trichloro-3,3,3-tri-fluoro-] (Note 3) is added in portions through the condenser. A mild exotherm results, and the addition is extended over ca. 5 minutes to... 

Tri-O-acetyl-a-D-xylopyranosyl bromide106 (138) and N-tosyl-L-serine methyl ester107 (139) were condensed in the presence of Drierite and silver oxide, and then the O-acetyl and methyl ester groups were removed by treatment with sodium hydroxide, and the N-tosyl group by means of sodium in liquid ammonia, to give 140. Synthesis of this compound has also been described by other workers108-110 and the a-D an-omer by Brendel and Davidson.108... 

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