1-METHYL-2-QUINOLINONE synthesis
- Product Name:1-METHYL-2-QUINOLINONE
- CAS Number:606-43-9
- Molecular formula:C10H9NO
- Molecular Weight:159.18
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Yield:606-43-9 98.1%
Reaction Conditions:
Stage #1:2-methylquinoline with 2-monochlorophenol;water at 26; for 2 h;
Stage #2: with iridium(IV) oxide;potassium chloride at 35; for 2 h;Temperature;
Steps:
3 Example 3:The method for synthesizing the pharmaceutical intermediate 1-methyl-2-quinolinone comprises the following steps:
A: 3 mol of 2-methylquinoline and 800 ml of a 37% by mass solution of 2-chlorophenol were added to the reaction vessel.Control the solution temperature to 26 ° C, add 9 mol aqueous solution, 1.2 L mass fraction of 16% butane solution, control the stirring speed230 rpm, reaction 120 min;B: Then add 600ml of a 25% potassium chloride solution, 8mol of iridium dioxide powder, and raise the temperature toAt 35 ° C, the reaction was continued for 2 h, the temperature was lowered to 9 ° C, the solution was layered, and the oil layer was washed with a sodium nitrate solution having a mass fraction of 11%.50min, a mass fraction of 78% diglyme solution for 40min, in a mass fraction of 86% sulfolane solutionThe medium recrystallized and dehydrated activated alumina were dehydrated to obtain 467.937 g of the finished 1-methyl-2-quinolinone, and the yield was 98.1%.
References:
Chengdu Kadifu Technology Co., Ltd.;Liao Runai CN108239027, 2018, A Location in patent:Paragraph 0016-0027
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