ChemicalBook CAS DataBase List 2-Chloro-4,6-dinitroaniline

2-Chloro-4,6-dinitroaniline synthesis

11synthesis methods

Product Name:2-Chloro-4,6-dinitroaniline
CAS Number:3531-19-9
Molecular formula:C6H4ClN3O4
Molecular Weight:217.57

97-02-9
7 suppliers
$10.00/25g

3531-19-9
160 suppliers
$16.00/25g

Yield:3531-19-9 98.4%

Reaction Conditions:

Stage #1:2,4-Dinitroanilin with hydrogenchloride in water at 35; for 2 h;
Stage #2: with chlorine in water at 45;
Stage #3: with dihydrogen peroxide in water at 60 - 65; for 6 h;Temperature;

Steps:

1-2
350 g of 2,4-dinitroaniline with a content of 99.86% after colloid milling,700 grams of hydrochloric acid with a mass concentration of 31% and 500 grams of water are added to the reactor,The temperature was raised to 35±5°C and stirred for 2 hours.Add 83 grams of chlorine gas to the reaction kettle, the temperature is controlled at 45 ± 5 ;Within 4~5 hours, chlorine gas is added completely; then keep at 45±5 for 2 hours.After 2 hours of incubation,Increase the temperature of the reaction kettle to 60±5, then start to dropwise add 96g of hydrogen peroxide with a concentration of 27.5%, and the temperature is controlled at 65±5.After the addition of hydrogen peroxide is completed within 4 hours; after the completion of the dropwise addition, the reaction is held at 65°C±5°C for 2 hours, and 513 grams of wet product is obtained after suction filtration.After drying, 409 g of product with 98.3% HPLC content was obtained, the product yield was 98.4%, and 1210 g of hydrogen chloride containing 17.78% concentration was obtained.A mother liquor with a hydrogen peroxide concentration of 0.022%, all 1210 grams of the mother liquor are recycled.

References:

Henanluo Dyeing Co., Ltd.;Ding Xiangbo;Duan Xiaoning;Feng Dongxing;Su Fengli;Peng Chuanyun;Xu Guozhan;Duan Xingwei;Yang Wei;Liu Jinfu;Ren Qinzhang;Qiu Shuntong;Liu Qing CN110963925, 2020, A Location in patent:Paragraph 0027-0032