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ChemicalBook CAS DataBase List 2-Nitroacetophenone

2-Nitroacetophenone synthesis

9synthesis methods
o-Nitroacetophenone is synthesized from o-nitroethylbenzene by oxidation. Add o-nitroethylbenzene, decanoic acid and initiator azobisisobutyronitrile into the reaction tower, and at the same time slowly pass air into the tower, keep the pressure at 0.3-0.8MPa, and control the oxidation at 120-130°C to generate 2-Nitroacetophenone.
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Yield:577-59-3 97%

Reaction Conditions:

with calcium silicate;sulfuric acid;nitric acid at -15;

Steps:

1.1 Step 1: Synthesis of 2'-nitroacetophenone
100 g of acetophenone is slowly added into a mixture of 500 ml of sulfuric acid and nitric acid (concentrated sulfuric acid and concentrated nitric acid in a volume ratio of 1:7 and a temperature of -15°C), and then 90 g of calcium silicate powder (14 g) is added (acetophenone and silicic acid). The weight ratio of calcium powder is 1:0.14).Keep stirring below -15°C overnight, then add ice water and filter to obtain 2-nitroacetophenone 134g as a yellow solid, yield 97%, purity 99.8%, MS: m/z=165 (M+), elemental analysis: C58.1% (theoretical 58.2%), H4.2% (theoretical 4.2%), O 29.0% (theoretical 29.1%), N8.4% (theoretical 8.5%), confirmed by molecular weight and elemental analysis 2'-nitroacetophenone.

References:

Shanghai Titan Technology Co., Ltd.;Xie Yingbo;Zhang Qing;Zhang Hua;Xu Xiaobing;Luo Guiyun CN105198813, 2018, B Location in patent:Paragraph 0016; 0019; 0020

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