ChemicalBook CAS DataBase List 3-AMINO-1,2,4-BENZOTRIAZINE-1,4-DIOXIDE

3-AMINO-1,2,4-BENZOTRIAZINE-1,4-DIOXIDE synthesis

8synthesis methods

Product Name:3-AMINO-1,2,4-BENZOTRIAZINE-1,4-DIOXIDE
CAS Number:27314-97-2
Molecular formula:C7H6N4O2
Molecular Weight:178.15

480-96-6 Synthesis

480-96-6
186 suppliers
$10.00/1g

420-04-2 Synthesis

420-04-2
340 suppliers
$15.00/25g

27314-97-2
143 suppliers
$45.00/10mg

Yield:27314-97-2 60%

Reaction Conditions:

Stage #1:benzofurazan oxide;CYANAMID with sodium hydroxide in methanol;water at 60; for 4 h;
Stage #2: with acetic acid; pH=5 - 8

Steps:

1 Preparation of 3-amino-1,2,4-benzotriazine-1,4-diazonium oxide
Benzofurazan weighed 27.2g (0.2 mol) and 25.2g solid Cyanamide(NH2CN, 0.6 mol) was placed in a 500 ml three-necked flask and dissolved in 200 ml of 50% aqueous methanol solution.Stir and slowly add sodium hydroxide 48g (1.2mol) until sodium hydroxide is added.The reaction was placed in a 60°C water bath and TLC traced the reaction until the end of the reaction (4 h). During the reaction, the solution slowly turned purple-black, cooled, filtered, and the filter cake was dissolved in an appropriate amount of water and then filtered. The mother liquor was collected and acidified with acetic acid. The pH is 5-8, the red solid material is obtained, DMF is crystallized and recrystallized, filtered, and dried to obtain the target compound 24.5g, yield 60%

References:

The Chinese People's Liberation Army Military Academy Of Medical Sciences Radioactive And Radiation Medical Institute;Huang Rongqing;Xiao Bingkun;Yang Jianyun;Ding Rui;Wu Gang CN102887869, 2018, B Location in patent:Paragraph 0041-0043

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