9-CHLORO-2-METHYLACRIDINE synthesis

12synthesis methods

Product Name:9-CHLORO-2-METHYLACRIDINE
CAS Number:16492-09-4
Molecular formula:C14H10ClN
Molecular Weight:227.69

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Yield:16492-09-4 98%

Reaction Conditions:

with trichlorophosphate at 85 - 135; for 2 h;Concentration;Temperature;

Steps:

1.2 Step two,

in a 100 ml round-bottom flask, add 18mmol compound a and 14.37 ml phosphorus oxychloride, oil bath, the temperature stages, first heating to 85 °C, the violent reaction occurs, immediately the other removed, if the reaction is too violent, using cold water cooling the flask, and then continue to slow to be boiling temperature to 135 °C reaction, 2h after removing excess phosphorus oxychloride is distilled under reduced pressure, the crude product obtained after 2nd, cooling, the 2nd adding concentrated crude product in a mixture of ammonia and chloroform, the holding concentrated ammonia and chlorofrom mixture in the container is arranged in the ice bath, for a mixture of concentrated ammonia water and chloroform washing burn bottle, 2nd with the washing liquid containing the concentrated crude product mixture of ammonia and chloroform, 30 min after all to be 2nd after dissolving crude product, chloroform level separated, water layer continue to use chloroform extraction, the extraction of the merger chloroform level two times with anhydrous calcium chloride drying, 24h after-filtration, evaporate the solvent, get strawcoloured powder, that is, for the compound b, the yield is 98%;

References:

CN105481847,2016,A Location in patent:Paragraph 0033

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118-91-2 Synthesis

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