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ChemicalBook CAS DataBase List 6-Bromo-1-methyl-1H-indazole
590417-94-0

6-Bromo-1-methyl-1H-indazole synthesis

5synthesis methods
-

Yield: 85%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl acetamide;water at 100; for 40 h;Industrial scale;Reagent/catalyst;Temperature;Solvent;

Steps:

1.1; 2.1; 3.1; 4-9; 10.1
(1) Add 3000.0 ml of N,N-dimethylacetamide to the reaction flask.2-fluoro-4-bromobenzaldehyde 1500.0 g (7.39 mol, 1.00 equ.), cooled to 0 ° C,Add 1530.0 g of potassium carbonate (11.10 mol, 1.50 equ.), and then add 3000.0 ml of methyl hydrazine (40 wt.% aqueous solution) dropwise. After the addition, the temperature was raised to 100 ° C, and the reaction was carried out for 40 hours.The raw material was completely reacted, cooled to room temperature, extracted with ethyl acetate and water, and layered.The organic phase was washed with 2M aqueous hydrochloric acid solution and 7% aqueous sodium hydrogencarbonate solution and brine, and the organic phase was concentrated, n-heptane crystals, filtered, and the cake was dried at 40 ° C for 22 hours.Obtaining 1320.0 g of 6-bromo-1-methylcarbazole,Yield: 85%.

References:

Shaoyuan Science And Technology (Shanghai) Co., Ltd.;Qidong Shaoyuan Chemical Technology Co., Ltd.;Yang Jun;Xue Duoqing;Wu Yong;Chen Lihuang;Zhai Lianhua CN110128347, 2019, A Location in patent:Paragraph 0046-0049; 0055-0057; 0064-0066; 0073-0084; 0089

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