ChemicalBook CAS DataBase List 2-Nitrobenzyl bromide

2-Nitrobenzyl bromide synthesis

6synthesis methods

Product Name:2-Nitrobenzyl bromide
CAS Number:3958-60-9
Molecular formula:C7H6BrNO2
Molecular Weight:216.03

88-72-2
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$15.00/25g

3958-60-9
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$8.00/1g

Yield:3958-60-9 98.5%

Reaction Conditions:

Stage #1:1-methyl-2-nitrobenzene with 2,2'-azobis(isobutyronitrile) in 1,2-dichloro-ethane for 0.333333 h;
Stage #2: with hydrogen bromide;dihydrogen peroxide in 1,2-dichloro-ethane at 72 - 75; for 2 h;Solvent;Temperature;

Steps:

2
In a 5000-L bromination reactor, 300 kg of dichloroethane, 226 kg of o-nitrotoluene, and 27 kg of azobisisobutyronitrile are successively added. After stirring for 20 minutes, the solution is pumped into a high tank for use; and the bromination reactor is put in again. 300 kg of dichloroethane and 226 kg of o-nitrotoluene were mixed well, and 889.03 kg of 40% hydrobromic acid was added, and the mixture was stirred at a temperature of 72 to 75°C. In the upper slot The mixed solution and 448.26 kg of 30% hydrogen peroxide were slowly added dropwise to the bromination reactor at an acceleration of 1:4. At the end of the addition, the reaction was continued for 2 hours. After the reaction was completed, the temperature was lowered to room temperature, and the reaction liquid was subjected to HPLC analysis. The conversion of the raw material was greater than 99.0%, and no by-product such as dibrominated product was generated. The molar ratio of raw material, 40% hydrobromic acid and 30% hydrogen peroxide in the reaction is 1: 1.2:1.2. The solution was allowed to stand for delamination and the upper aqueous layer was separated; after the lower organic phase was washed with 600 L of water, the solvent was distilled off under reduced pressure and rinsed with cold dichloroethane to obtain white o-nitrobenzyl bromide solid product. It is 98.5%.

References:

Zhejiang Zhongshan Chemical Group Co., Ltd.;Li Jing;Wang Tao;Chen Lu;Yu Ronghua CN107778181, 2018, A Location in patent:Paragraph 0008; 0028; 0029

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612-25-9 Synthesis