ChemicalBook CAS DataBase List 2,3-DINITROTOLUENE

2,3-DINITROTOLUENE synthesis

15synthesis methods

Product Name:2,3-DINITROTOLUENE
CAS Number:602-01-7
Molecular formula:C7H6N2O4
Molecular Weight:182.13

570-24-1 Synthesis

570-24-1
360 suppliers
$6.00/10g

602-01-7
47 suppliers
$35.20/250mg

Yield: 86.8%

Reaction Conditions:

with sodium perborate;titanium(IV) hydroxide;acetic acid at 90 - 100; for 1 h;Inert atmosphere;

Steps:

6 Example 6
Three to 500ML bottle with reflux condenser tube was added 216g of glacial acetic acid, stirred open, thenWas added sodium perborate and 57g 5g titanate prepared in Example 1 of the catalyst, the air inside the system was replaced with nitrogenThree times, heated to 90 deg.] C, was added dropwise 10g2- methyl-6-nitroaniline and 30g of acetic acid with stirringThe mixed solution, and then 90 ~ 100 reaction was stirred 1h. The progress of the reaction by TLC, the reaction was completeAfter a, the system was lowered to room temperature, suction filtered, and the resulting solid was washed with 20g of methanol, and 40 ~ 50 3 hours and dried in vacuo to give methyl 1,6-dinitrobenzene 11g2-, purity 96%, yield 88%.The preparation of 2-methyl-1,6-dinitrobenzene was added to the crude product 35g absolute ethanol, warmed to 75 ~ 80 reflux for 1h, then cooled system to 0 ~ 5 , keep stirring 1h, filtration, solid 40 ~ 50 3h and dried in vacuo to give methyl 1,6-dinitrobenzene 10.5g2- pure, purity 99.2%, yield86.8%.

References:

Jinan Kabo Tang Biotechnology Co., Ltd.;Meng, Qingwen;Xi, Zunbo;Li, Dachuan;Wang, Wubao;Ning, Shuguang;Cheng, Jingwei;Gu, Zhenlei CN104086429, 2016, B Location in patent:Paragraph 0049; 0050; 0051