Brown extractor

Several types of Brown extractors are used in the citrus industry throughout the world. The Model 400 produces a juice that is low in peel oil content and high in juice quality. The fruit is halved and the juice removed by a rotating reamer that exerts pressure to effect extraction. 

B. 2-Methylcyclopenlane-l,3,5-trione hydrate. A mixture of 200 g. (0.89 mole) of the keto ester prepared above, 910 ml. of water, and 100 ml. of 85% phosphoric acid is healed under reflux for 4 hours and then cooled in an ice-salt bath to —5°. The trione mixed with oxalic acid separates and is collected by filtration and dried under reduced pressure. The dried material is extracted with boiling ether (250-300 ml.) under reflux, and the ethereal extract is separated from the undissolved oxalic acid. The original aqueous filtrate is also extracted with ether in a continuous extractor. The two extracts are combined, and ether is removed by distillation. The crude trione separates as a dark brown solid and is crystallized from ca. 250 ml. of hot water. The once-crystallized, faintly yellow product weighs 95-105 g. (74-82%), m.p. 70-74°. This product is used in the next step without further purification. A better specimen, m.p. 77-78°, which is almost colorless, can be obtained by recrystallization from hot water after treatment with Norit activated carbon. 

Under N2, clean Li metal (0.17 g, 25 mmol) was placed in a round-bottom flask with a solvent mixture of MeOH (3 mL) and pcntan-t-ol (17 mL). The mixture was heated under N, until the reaction with Li was complete. Then, naphthalene-2,3-dicarbonitrilc (2 g, 11 mmol) was added to the mixture which turned green-brown the mixture was refluxed for 3h. The brown powder, obtained after cooling and removal of the solvent under reduced pressure, was dissolved in anhyd acetone (20 mL) and then hexane (70 mL) was added. The green precipitate was separated from the brown solution by filtration. This purification by precipitation was repeated twice. The green precipitate was placed in a Soxhlet extractor and extracted for 3 h with acetone (200 mL) in order to separate the product from the insoluble metal-free species and LiOH. The acetone solution was evaporated down to a volume of 20 mL. The product precipitated after the addition of hexane (70 mL). This latter purification step was performed several times yield 1.29 g (64%). 

Noth NA — not analyzed — none detected x — none detected, but brown precipitate was recovered from the extractor upon cleaning. 

The Brown Model 700 Extractor operates in a manner similar to the Model 400 and produces juice of the same high quality with low oil content. It expresses the juice from about 700 fruit/min. compared to the 350 fruit/min. that can be processed by the Model 400. 

The tocopherol content of midseason orange oils followed the order Brown peel shaver (216 ppm), FMC in-line extractor (126 ppm) and screw press (104 ppm). The method of extraction influenced both the evaporation residue and the tocopherol content of orange oil, the higher the evaporation residue, the higher the tocopherol content. Since tocopherol is a good antioxidant,... 

Liquid Carbon Dioxide Extraction. Mature ginger (Z. officinale Roscoe) rhizomes were obtained from a supplier in Hsinchu (Taiwan). The rhizomes were washed, sliced, freeze-dried, ground and sieved (200 mesh). About 110 g of freeze-dried ginger powder was placed in a glass Soxhlet extractor installed in a stainless steel liquid carbon dioxide extractor. Operating procedures were described previously (13). A golden brown oil material (3.44%) was obtained by the liquid carbon dioxide extraction. 

TetramethyIisoindole (6 g, 34.6 mmole) and cobalt powder (30 g, 0.51 mole) are mixed and loaded into a Carius tube (4 X 35 cm volume about 450 mL). After it is evacuated and sealed, the tube is placed in a shielded oven preheated to 390° and heated at this temperature for 4 hours. After the tube is cooled, the dark-blue (or black) powder is placed in a Soxhlet extractor and extracted with pentane (300 mL) until a red-brown impurity is removed (about 24 hours). The pentane is replaced by toluene (300 mL), and extraction is continued until the extract (initially green) is colorless (about 8 hr). Finally, pyridine (300 mL) is used to extract (Soxhlet extractor) the porphine, which requires about 10 hours. The pyridine solution is concentrated to 20 mL, and 100 mL of hexane is added. The precipitate is collected, washed with hexane, and dried overnight in vacuum at 60°, to give [octamethyltetrabenzoporphinato-(2-)] cobalt(II). Yield 2-3 g (35-55%). Anal. Calcd. for C44H36N4Co C, 77.79 H, 530 N, 8.24. Found C, 77.87 H, 5.40 N, 8.48. 

Hydrazine hydrate (29.4 mL, 30.32 g, 0.61 mole) is added dropwise from a pressure-equalizing addition funnel to a cooled (0°) solution of hexachloro-1,3-cyclopentadiene (16 mL, 27.3 g, 0.10 mole) in 200 mL of methanol in a 500-mL Erlenmeyer flask. The solution turns dark red immediately. After the addition, the flask is securely stoppered (with a glass stopper) and the solution is stirred in the dark for 5 days at 5°, during which time a red solid collects on the walls of the flask. The mixture is poured into 5 L of water and filtered. The solid is air dried, dissolved in diethyl ether, and filtered. The filtrate is evaporated to dryness and the residue is extracted with cyclohexane in a Soxhlet extractor. The solution is concentrated and cooled and the red-brown crystals are filtered off. Additional product can be obtained by washing the material remaining in the thimble with water and extracting again with cyclohexane. Total yield 15 g (65%). 

Powdered crystals of EBA (200 mg) were placed in a 100-mL round-bottomed flask and heated in an oil bath at 115 °C (A), and at 125 °C (B), under N2 for 3 days. The dark reddish-brown colored products were then extracted for 3 days in a Soxhlet extractor using toluene to remove the unreacted monomer. The products were vacuum dried at 60°C for 7-10 days yielding (A 34%, B 42%) red (A) and orange (B) powders entirely free of monomer and toluene. NMR and GPC analysis of the thermal products indicated that A consisted of pure PCPA, whereas B consisted of a near-equal mixture of TCPB and PCPA. 

B21a. Brown, J. B., Macleod, S. C., MacNaughtan, C., Smith, M. A., and Smyth, B., A rapid method for measuring oestrogens in human urine using a semiautomatic extractor. J. Endocrinol. 42, 5-15 (1968). 

Continuing to exclude all air and water, the residue is loaded into a Soxhlet extractor. All joints are fitted with Teflon sleeves. The residue is extracted with pentane (150 mL) for 2 days or until the residue becomes white and the solution is reddish brown. The volatiles are removed from the solution to afford the product as a brown solid in 66% yield (3.2 g). mp 80-82°C. 

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