1196107-73-9 synthesis
- Product Name:1196107-73-9
- CAS Number:1196107-73-9
- Molecular formula:C23H15BrO2
- Molecular Weight:403.27
![2-[(7-bromo-9,9-dimethyl-9H-fluoren-2-yl)carbonyl]Benzoic acid](/CAS/20211123/GIF/1196107-72-8.gif)
1196107-72-8
1196107-73-9
General procedure: 2-Bromo-9,9-dimethyl-7-(2-carboxybenzoyl)fluorene (20 g, 0.047 mol, 1 eq.) was used as a raw material, which was placed in a reaction flask and polyphosphoric acid (50 ml) was added. The reaction mixture was heated to 140 °C for the reaction. After completion of the reaction, the resulting solid product was filtered, washed with a small amount of methanol and then dried to afford the target compound 2-bromo-13,13-dimethyl-6H-indeno[1,2-b]anthracene-6,11(13H)-dione (16.6 g, 81% yield). The product was characterized by 1H-NMR: δ 8.29 (t, 2H), 8.09 (s, 2H), 7.85 (d, 2H), 7.72 (m, 3H), 1.67 (s, 6H).
85-44-9
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28320-31-2
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1196107-73-9
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$13.00/100mg
Yield: 73.6%
Reaction Conditions:
Stage #1:phthalic anhydride;2-bromo-9,9-dimethyl-9H-fluorene with aluminum (III) chloride in dichloromethane at 0; for 6 h;Inert atmosphere;
Stage #2: with phosphoric acid at 130; for 3 h;
Steps:
1 (1) Synthesis of Intermediate 1-2
Nitrogen gas was introduced into a 2L three-necked flask, and 1 L of dichloromethane was sequentially added.53.7 g of aluminum trichloride, cooled to 0 ° C, then added 100 g of intermediate 1-1,After stirring, the raw material was completely dissolved, and then a solution of 54.3 g of phthalic anhydride in 200 ml of DCM was added dropwise;After the completion of the dropwise addition, the reaction was continued for 6 h, and TLC monitored that the intermediate 1-1 was completely consumed, and the reaction was stopped; the reaction solution was poured into a cold 6 M hydrochloric acid solution.After thorough stirring, the liquid phase is statically separated, and the organic phase is washed with water until neutral. After drying with anhydrous sodium sulfate, the white solid obtained is concentrated and added to 400 ml of phosphoric acid, and heated to 130 ° C to stir the reaction for 3 hours;At room temperature, the reaction solution was poured into ice water, and sodium hydroxide solution was added to adjust the pH to neutral.Filtration, the filter cake is washed to neutral; the filter cake is dried and then purified by methanol.108.6g of pale yellow solid, ie intermediate 1-2,The yield was 73.6%.
References:
Xi'an Ruilian New Materials Co., Ltd.;Sun Jun;Zhang Hongke;Liu Kaipeng;Tian Mi;Yang Dandan;He Haixiao;Li Jiangnan;Wang Xiaowei;Liu Qianfeng;Gao Renxiao CN110041366, 2019, A Location in patent:Paragraph 0075-0078
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1000210-73-0
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1196107-73-9
94 suppliers
$13.00/100mg
28320-31-2
308 suppliers
$5.00/1g
1196107-73-9
94 suppliers
$13.00/100mg
28320-32-3
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$6.00/1g
1196107-73-9
94 suppliers
$13.00/100mg