Reduction apparatus

A mixture of ethyl cyanoacetate (Note 1) (56.6 g., 0.5 mole), freshly distilled butyraldehyde (43.2 g., 0.6 mole), 1 g. of palladium on carbon (Note 2), and 80 ml. of glacial acetic acid is placed in a 500-ml. bottle suitable for attachment to a low-pressure reduction apparatus. A solution of piperidine (2.0 ml., 0.02 mole) in 20 ml. of glacial acetic acid is added, and the bottle is connected to the reduction apparatus. 

Other forms of catalytic reduction apparatus which may be used in the laboratory have been described in the following articles.1... 

A solution of 20.8 g. (0.1 mole) of benzalacetophenone (Note 1) (Org. Syn. 2, 1) in 150 cc. of c.p. ethyl acetate (Note 2) is placed in the reaction bottle of the catalytic reduction apparatus (p. 10) and 0.2 g. of platinum oxide catalyst (p. 92) is added. The apparatus is evacuated, then filled with hydrogen, and the mixture shaken with hydrogen until 0.1 mole has been absorbed. The time required is usually about fifteen to twenty-five minutes (Note 3). The platinum is filtered off and the solvent removed from the filtrate by distillation. The benzylacetophenone is recrystallized from about 25 cc. of alcohol and melts at 72-730. The yield is 17-20 g. (81-95 per cent of the theoretical amount). 

A schematic of this high temperature reduction apparatus is shown in Figure 4. 

Electrolytic reduction, apparatus, 52, 23 Enol acetates, acylation of, 52,1 Enol esters, preparation, 52, 39 Epichlorohydrin, with boron trifluoride diethyl therate and dimethyl ether to give trimethyloxonium tetra-fluoroborate, 51,142 ESTERIFICATION OF HINDERED ALCOHOLS f-BUTYL p-TOLUATE,... 

Figure 1. (a) The zeolite dehydration apparatus (b) the zeolite reduction apparatus... 

Raney Nickel Reduction Apparatus in Appendix IIIC under Sulfur by Oxidative Microcoulometry). On top of the boiling flask, fit a water-jacketed distillation column with hooks. To the distillation column, fit a piece of glass tubing with ground ST inner joints with hooks, and connect the distillation column and a gas dispersion tube with ST outer joints with hooks. 

Fig. 6. A schematic diagram of the reduction apparatus for the production of metallic europium...

See Amphetamine Syntheses Industrial for a detailed description of the electrolytic reduction apparatus. 

Method B 180 g tropine or pseudotropine is dissolved with 70 g ammonium sulphate in 720 g water, on which sulfuric acid up to the neutralization is added. This solution is made alkaline with ammonia poured into the anode region of the electrolytic reduction apparatus, while in the cathode area a solution of 280 g ammonium sulfate in 800 g water. The further procedure is then exactly the same, as described 1 in the example. Source Merck 1901... 

Schmieder(5) said that in the presence of hydrazine in a common cathode-anode space, there happens only the formation of U(IV) on the cathode without any reoxidation of it on the anode until the course of electrolysis reaches the stage of oxygen evolution on the anode. He said that this is due to the fact that oxidation of U(IV) has a high oyerpotential on the anode. Then it should be possible to construct an electrolytic reduction apparatus without a diaphragm. 

It may be necessary to warm the mixture in order to dissolve the acetaminocinnamic acid completely in this amoimt of acetic acid. In this case the solution should be allowed to cool to room temperature before it is placed in the reduction apparatus. 

A SOLUTION of 20.5 g. (o.i mole) of a-acetaminocinnamic acid (p. i) in 150 cc, of glacial acetic acid (Note i) is placed in the bottle of a Burgess-Parr reduction apparatus, 0.5 g. of platinum oxide catalyst (Org. Syn. Coll. Vol. I, 452 17, 98) is added, and the mixture shaken in an atmosphere of hydrogen under an initial pressure of 40 lb. per sq. in. until the calculated amount of gas is taken up usually about two hours is required (Notes 2 and 3). When the reduction is complete, the catalyst is removed by suction filtration and washed with a little water. The combined filtrate and washings are evaporated to dryness under diminished pressure on a water bath. 

Sne electrolytic reduction apparatus as described in Airiphetamine Syntheses. 

Gas At a Polystyrene Foam reprocessing plant. Blowing Agent Gas was accumulated caused by the choke of closed type volume reduction apparatus in operation, and explosion broke out due to static electrical spark ignition... 

The range of applications of size reduction is very wide. It includes the preliminary breakup of large masses into pieces that can be handled in a process and the grinding of smaller particles into fine powders. The size and design of equipment reflect this situation. Broadly, size reduction apparatus can be divided into those types which depend on mechanical crushing and those which use impact to fracture the solids. Table 3-13 shows some of the common types of equipment with their principal characteristics. Major hazards are those associated with the machinery and with the material being processed. 

Fig. VII-1 Hydrogen reduction apparatus as used by Hofmann and Schneider (75)...

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