Glass autoclaving

Low pressure hydrogenator equipped with a 500 mL glass autoclave, a heater, and a magnetic stirrer... 

In a glass autoclave equipped with a magnetic stirrer bar were placed BisP -RuBr2 (52 mg), methyl 3-oxopentanoate (10.7 g), and degassed methanol/ water (10/1) 200 mL under an argon atmosphere. 

Caution. Carbon monoxide is an odorless, colorless and very toxic gas. The reaction must be conducted in a well-ventilated fiime hood. The glass autoclave must be covered by a protection cage during the work with carbon monoxide under pressure. 

Similarity reaction of vinyl chloride with phenylacetylene in diethylamine using dichloro[bis(diphenylphosphino)ethane]palladium (II) and copper(I) iodide as a catalyst and a glass autoclave as a reaction vessel afforded 4-phenylbut-l-en-3-yne in 85% yield. 

The glass autoclave nwst be used with appropriate precaution. A pressure of about 20 p.s.1. Is generated, so a low positive pressure reactor, such as a shielded Flscher-Porter Bottle (Fischer and Porter Company, Lab-Coest Division, Warminster, PA 18974), can be used Instead. Alternatively the reaction may be carried out without pressure equipment In 3 days. 

The Slurry Polymerization Process with Super-Active Ziegler-Type Catalyst Systems From the 2 L Glass Autoclave to the 200 m Stirred Tank Reactor... 

The polymerization reaction is carried out in a 1 L flat-flanged glass autoclave. The four-necked flat top carries a condenser, a nitrogen inlet, a thermocouple, and a stirrer. Due to the high viscosity of the reaction mixture, the stirrer and the thermocouple should be made of steel. Heating can be done in a (transparent) oil bath that allows observation of the reaction. 

With suitable safety precautions and by techniques similar to those of Preparation 3-3, a 1.5-liter stirred glass autoclave (Ingenieurbiiro S.F.S., Zurich) is charged with 750 ml of deionized and deaerated water, 0.525 gm of Methocel 90 HG/100 cP (Dow Chemical Co.), 0.1125 gm of Tensaktol A (B.A.S.F.), and 0.6 gm of lauroyl peroxide. The reactor is sparged with nitrogen, evacuated, then charged with 375 gm of vinyl chloride and closed. 

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