9,9-dimethylcarbazine synthesis
- Product Name:9,9-dimethylcarbazine
- CAS Number:6267-02-3
- Molecular formula:C15H15N
- Molecular Weight:209.29
73183-55-8
6267-02-3
General procedure for the synthesis of 9,9-dimethyl-9,10-dihydroacridine from the compound (CAS: 73183-55-8): 80 g (0.35 mol) of the compound obtained in the previous step was added to 1.7 L of phosphoric acid and the reaction mixture was stirred for 12 hours at room temperature. After completion of the reaction, the reaction mixture was neutralized with distilled water, the resulting solid was filtered and washed with distilled water. The solid was dissolved in dichloromethane, extracted and subsequently neutralized with sodium hydroxide solution. The organic layer was dried with magnesium sulfate and the solvent was removed by rotary evaporator. Finally, purification by recrystallization in hexane afforded 64 g of 9,9-dimethyl-9,10-dihydroacridine in 87% yield.
35708-19-1
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75-16-1
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6267-02-3
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Yield:6267-02-3 81%
Reaction Conditions:
in tetrahydrofuran at 0;
Steps:
1.2 Synthesis of intermediate product (B)
20.0 g (88.00 mmol) of the intermediate (A) synthesized in the above step 1 was suspended in terrahydrofuran (293 ml), and then 102.7 ml of methylmagnesium bromide (3M) was slowly added dropwise at 0 ° C. After completion of the reaction, the reaction solution was extracted with dichloromethane and distilled under reduced pressure. 100 ml of sulfuric acid diluted to 10% in distilled water was added to the distillation product, and the mixture was stirred at room temperature for 12 hours. After completion of the reaction, the reaction mixture was extracted with dichloromethane and distilled water, and the organic layer was subjected to silica gel filtration. The organic solution was removed and recrystallized from dichloromethane and hexane to obtain 15.0 g (yield: 81%) of the intermediate product (B).
References:
Cheil Industries Co., Ltd.;Yoo, Dong Kyu;Yoo, Eun Sun;Lee, Han Ir;Jung, Sung Hyun;Hao, Dal Ho;Hong, Jin Suk;Ryu, Dong Wan;Chae, Mi Young KR2016/102142, 2016, A Location in patent:Paragraph 0215; 0223; 0224
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6267-02-3
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38158-59-7
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112817-88-6
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6267-02-3
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