ChemicalBook CAS DataBase List 1,2,3,4-Tetrachlorobenzene

1,2,3,4-Tetrachlorobenzene synthesis

7synthesis methods

Product Name:1,2,3,4-Tetrachlorobenzene
CAS Number:634-66-2
Molecular formula:C6H2Cl4
Molecular Weight:215.89

634-67-3 Synthesis

634-67-3
79 suppliers
$35.00/1g

634-66-2
118 suppliers
$20.89/100mg

Yield:634-66-2 82%

Reaction Conditions:

Stage #1:2,3,4-trichloroaniline with hydrogenchloride;sodium nitrite in water at -5 - 5; for 1 h;Sandmeyer Reaction;
Stage #2: with copper(l) chloride in water at 50 - 80; for 1 h;Sandmeyer Reaction;

Steps:

3 Preparation of intermediate 1,2,3,4-tetrachlorobenzene (IV)
In a 500 ml bottle 2,3,4-trichloroaniline 10 g (0.051 mol) and concentrated hydrochloric acid 21 g were added. The temperature was controlled to -5-5°C by adding 4 g of aqueous solution of sodium nitrite. After completion of addition, the mixture was insulated for 1 hour. In another 1000 ml bottle 50 g concentrated hydrochloric acid and 6 g cuprous chloride were added at 50°C and the preceding nitrosation solution was added, and heated to 80°C for 1 hour. Then the mixture was cooled to 30 ° C, extracted with dichloroethane, and evaporated to dryness to obtain 1,2,3,4-tetrachlorobenzene 9 g, GC analysis (more than 98%) yield of 82%.

References:

Shanghai North Carolina Pharmaceutical Technology Co., Ltd;Wang, Yong;Liu, Ligang;Zhang, Wujun;Sun, Jing;Li, Qian;Huang, Junjie;Xie, Jianfei;Kang, Litao CN105801429, 2016, A Location in patent:Paragraph 0105-0108

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117-08-8 Synthesis