Filtration brine

Bromo-2-nitrophenylacetic acid (26 g, 0.10 mol) was dissolved in a mixture of 50% HjSO (400 ml) and ethanol (600 ml) and heated to 90°C. Over a period of 1 h, zinc dust (26.2 g, 0.40 mol) was added. slowly and then heating was continued for 2 h. The excess ethanol was removed by distillation. The solution was cooled and filtered. The filtrate was extracted with EtOAc. The filtered product and extract were combined, washed with 5% NaCOj and brine and then dried (MgSO ). The solvent was removed in vacuo and the residue recrystallized from methanol to give 20.5 g (97% yield) of the oxindole. 

A solution of 2,3-dibromo-5-methoxyaniline (32 g, 0.17 mol) in CHjClj (300 ml) was stirred and cooled in an icc bath. Boron trichloride (1 M in CH2CI2, 180 ml, 0.18 mol), chloroacetonitrile (14.3 g, 0.19 mol) and TiC (1 M in CH CIj, 190ml, 0.19 mol) were added. The resulting mixture was refluxed for 1.5 h. The solution was cooled to room temperature and poured carefully on to a mixture of icc and 20% aq. HCl (700 ml). The organic layer was separated and the CH Clj removed by distillation. The residue was heated to 90°C on a water bath for 30 min. The solution was cooled and the solid collected by filtration. It was partitioned between ether (1.41) and 1 N NaOH (500 ml). The ether layer was washed with brine, dried over Na2S04 and evaporated. The residue was recrystallized from ethanol to give 2-amino-3,4-dibromo-6-methoxy-a-chloroacetophenone (55 g) in 90% yield. 

A mixture of l-(r-Boc)indol-2-yl-tri- -butylstannanc (1.2 mmol) and 4-bromo-benzonitrile (1.0 mmol) and Pd(PPh3)2C , (0.02 mmol) in dry dioxane (5 ml) was heated at I00°C overnight under nitrogen. The reaction mixture was cooled, diluted with EtOAc and stirred for 15 min with 15% aq. KF. The precipitate was removed by filtration and washed with EtOAc. The EtOAc layer was separated, washed with brine, dried (Na2S04) and concentrated. The residue was purified by chromatography on silica. The yield was 66%. 

The previous product was added to LiAlH (6 eq.) in THF. The solution was heated at reflux for 1 h. The excess hydride was destroyed by dropwise addition of water and the resulting mixture filtered through Celite. The filtrate was diluted with EtOAc, washed with brine and dried (Na2S04). The product was an oil (3.4 g, 98%). 

Among nonmetallic materials, glass, chemical stoneware, enameled steel, acid-proof brick, carbon, graphite, and wood are resistant to iodine and its solutions under suitable conditions, but carbon and graphite may be subject to attack. Polytetrafluoroethylene withstands Hquid iodine and its vapor up to 200°C although it discolors. Cloth fabrics made of Saran, a vinyHdene chloride polymer, have lasted for several years when used in the filtration of iodine recovered from oil-weU brines (64). 

Common names have been given to sodium sulfate as a result of manufacturiag methods. In rayon production, by-product sodium sulfate is separated from a slurry by filtration where a 7—10-cm cake forms over the filter media. Thus rayon cake was the term coiaed for this cake. Similarly, salt cake, chrome cake, phenol cake, and other sodium sulfate cakes were named. Historically, sulfate cakes were low purity, but demand for higher purity and controlled particle size has forced manufacturers either to produce higher quaUty or go out of busiaess. Sodium sulfate is mined commercially from three types of mineral evaporites thenardite, mirabilite, and high sulfate brine deposits (see Chemicals FROMBRINe). 

At Great Salt Lake Minerals Corporation (Utah), solar-evaporated brines are winter-chilled to —3° C in solar ponds. At this low temperature, a relatively pure Glauber s salt precipitates. Ponds are drained and the salt is loaded into tmcks and hauled to a processing plant. At the plant, Glauber s salt is dissolved in hot water. The resulting Hquor is filtered to remove insolubles. The filtrate is then combined with soHd-phase sodium chloride, which precipitates anhydrous sodium sulfate of 99.5—99.7% purity. Great Salt Lake Minerals Corporation discontinued sodium sulfate production in 1993 when it transferred production and sales to North American Chemical Corporation (Trona, California). 

North American Chemical Co. produces borax pentahydrate and decahydrate from Seades Lake brines in both Trona and West End, California (see Chemicals frombrines). The 88 km dry lake consists of two brine layers, the analyses of which are given in Table 11. Two distinct procedures are used for the processing of upper and lower lake brines. Borax is produced in Trona from upper lake brines by an evaporative procedure involving the crystallization of potash and several other salts prior to borax crystallization as the pentahydrate (104). A carbonation process is used in West End, California to derive borate values from lower lake brines (105). Raw lower stmcture brine is carbonated to produce sodium bicarbonate, which is calcined and recrystallized as sodium carbonate monohydrate. The borate-rich filtrate is neutralized with lake brine and refrigerated to crystallize borax. 

There are 10 producers of calcium chloride solutions in the United States, three of these also make a dry product. Solution production is centered around Michigan (brines), California and Utah (brines), and Louisiana (by-product acid). The majority of dry calcium chloride is made in Michigan, lesser quantities in Louisiana, and minor quantities in California. Production involves removal of other chlorides (primarily magnesium) by precipitation and filtration followed by concentration of the calcium chloride solution, either for ultimate sale, or for feed for dry product. Commercial dry products vary by the amount of water removed and by the nature of the drying equipment used. Production and capacity figures for the United States are indicated in Table 2. 

To a solution of m-ethyl cinnamate (44, 352 mg, 85% pure, 1.70 mmol) and 4-phenylpyridine-A-oxide (85.5 mg, 29 mol%) in 1,2-dichloromethane (4.0 mL) was added catalyst 12 (38.0 mg, 3.5 mol%). The resulting brown solution was cooled to 4°C and then combined with 4.0 mL (8.9 mmol) of pre-cooled bleach solution. The two-phase mixture was stirred for 12 h at 4°C. The reaction mixture was diluted with methyl-t-butyl ether (40 mL) and the organic phase separated, washed with water (2 x 40 mL), brine (40 mL), and then dried over Na2S04. The drying agent was removed by filtration the mother liquors concentrated under reduce pressure. The resulting residue was purified by flash chromatography (silica gel, pet ether/ether = 87 13 v/v) to afford a fraction enriched in cis-epoxide (45, cis/trans . 96 4, 215 mg) and a fraction enriched in trans-epoxide cis/trans 13 87, 54 mg). The combined yield of pure epoxides was 83%. ee of the cis-epoxide was determined to be 92% and the trans-epoxide to be 65%. 

B. Methyl indole-4-carboxylate (30). A mixture of 7.0 g (28 mmol) of methyl trans-2-[ -(dimethylamino)vinyl]-3-nitrobenzoate(29) in 140 mL of dry benzene which contained 1.4 g of 10% Pd/C was shaken in a Parr apparatus under Hj (50 psi) for 1.5 h. The catalyst was removed by filtration, and the benzene solution was washed with 30 mL of 5% aq. HCl, brine and dried over MgS04. After removal of the solvent under reduced pressure, the residue was purified via chromatography on silica gel to furnish 6.9 g (82%) of methyl indole-4-carboxylate (30). 

A fine suspension of 25.18 grams (0.05 mol) of potassium salt of enamine protected ampicillin and 10.65 grams (0.05 mol) 3-bromophthalide were reacted in a 1 2 mixture of acetone/ethyl acetate (1,500 ml) for 24 hours. After filtration the organic layer was washed twice with 250 ml portions of 1 N sodium bicarbonate and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. Addition of ether crystallized the phthalide enamine protected a-aminophenylacetamido penicillanate in 85% yield. 

Components in the invading water-based filtrate and in the formation waters may react to form insoluble precipitates which can block the pores and give rise to skin damage. The scale can be formed by interaction of calcium-based brines with carbon dioxide or sulfate ions in the formation water. Alternatively sulfate ions in the invading fluid may react with calcium or barium ions in the formation water. Analysis of the formation water can identify whether such a problem may arise. 

Brine-polymer systems are composed of water-salt solutions with polymers added as viscosifers or filtration control agents. If fluid loss control is desired, bridging material must be added to build a stable, low permeability bridge that will prevent colloidal partial movement into the formation. 

An injectivity test is performed using clean, solids-free water or brine. If a low fluid loss completion fluid is in the hole, it must be displaced from the perforations before starting the injecting. This test will give an idea of the permeability of the formation to the cement filtrate. 

A solution of 0.96g (2.4mmol) of (4,V,5,V)-4,5-dicyclohexyl-2-[(.S )-(Z)-l-mcthyl-2-butcnyl]-l,3,2-dioxa-borolane [(S,5,S)-7] in 5 mL of petroleum ether (bp 40 - 60 C) is treated with 0.35 g (2.4 mmol) of benzaldehyde for 12 h at r.t. The solution is then concentrated and taken up in 10 mL of diethyl ether. 0.35 g (2.4 mmol) of triethanolamine is added and the mixture is heated to reflux for 4 h. The resulting boratrane is filtered and washed with three 20-mL portions of diethyl ether. The filtrate is stirred intensively with 50 mL of 20% aq NaHS03, then the aqueous phase is extracted with two 20-mL portions of diethyl ether. The combined extracts arc washed with water and brine and then dried over MgS04. Concentration of this solution ill vacuo is followed by short-path distillation at 60 X/0.1 Torr yield 0.30 g (71%) 99% ee [chiral capillary GC on a (5)-valine-(5)-a-phenylethylamide column]39. 

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