ChemicalBook CAS DataBase List 5-BROMO-1,2,4-TRIMETHYLBENZENE

5-BROMO-1,2,4-TRIMETHYLBENZENE synthesis

11synthesis methods

Product Name:5-BROMO-1,2,4-TRIMETHYLBENZENE
CAS Number:5469-19-2
Molecular formula:C9H11Br
Molecular Weight:199.09

95-63-6
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$14.80/250mg

5469-19-2
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$26.39/25g

Yield: 97.3%

Reaction Conditions:

with sulfuric acid;dihydrogen peroxide;iodine;iron(II) sulfate;sodium bromide in dichloromethane;water at 0;

Steps:

1 Example 1
Weigh three toluene 0.1mol,0.15 mol of sodium bromide,30% sulfuric acid solution 0.08mol in three-necked flask,Then, 50 g of dichloromethane was added as a solvent,Add catalyst 0.8g ferrous sulfate,0.05g of iodine,The three-necked flask placed 0 low temperature tank, mixing, fully dissolved.A solution of 10% aqueous hydrogen peroxide (H2O, 20.08 mol) was added dropwise at 0 ° C over 3-5 hours,And incubated for 6 hours.The reaction is over, standing stratification,The organic phase was washed with 100 mL of water, repeated three times, and then the aqueous solution was extracted with 30 mL of dichloromethane, repeated three times. The organic phase solutions were combined,The methylene chloride was recovered under reduced pressure to give a crude solid product, which was recrystallized from twice the mass of gasoline to give white crystals,Is trimethylbenzene, about 19.4 g, yield 97.3%.

References:

Zhejiang Xinhecheng Pharmaceutical Co., Ltd.;Shangyu Xin He Cheng Biochemical Co., Ltd.;Zeng Qingyu;Xia Xiaozhong;Liu Xianghong;Zhu Xu;Lv Guofeng;Wang Lijian;Jiang Hengju;Huang Guodong CN106565423, 2017, A Location in patent:Paragraph 0013; 0028; 0029