Anonymous
09/22/2023 (Fri) 21:44
No.101044
del
>>100959Вот с саенсмеднеса репорт. Кому надо загоните в гугл переводчик
Phenylacetic acid from styrene, sulfur and ammonia
Autoclave volume 3L made from stainless steel tube 100mm diameter and wall thickness 5mm with MMA welding. Threaded tubes 1\2 welded to it. DO NOT USE COOPER AND ALUMINIUM ALLOYS FOR THIS SYNTESIS
Into autoclave put 500ml styrene 1100ml 25% ammonia 450 gr sulfur. After filling autoclave closed with wrench PTFE lent was used. Autoclave placed on water bath 95C at 5 days with break at night. Every 1-3 hours autoclave stirred by hands.
After 5 days at water bath autoclave was opened. Lower organic brown layer separated and washed with water. Autoclave washed with detergent.
In 1.3 liters of water dissolved 350 gr sodium hydroxide. Sodium hydroxide solution and autoclave tar placed to the stainless steel boiler with 1 meter 2/3 tube(reflux) and boiled 2 days with break at night.
After boiling in mixture added 300ml xylene and upper organic layer was separated. In water layer added 2 liters 15% hydrochloric acid
DANGER!!!Lots of hydrogen sulphide evaporated its jets are visible. In room all cooper things was turned black.
After filtration and washing 190gr wet impure phenylacetic acid was prepared. If after filtration acid water solution was extracted and saturated sodium chloride(50-100 gr liter) with toluene can be obtained about 10-20gr phenylacetic acid. Phenylacetic acid contaminated sulfur and needs in separation with ethanol as example.
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