ChemicalBook CAS DataBase List 4-Iodo-3-nitrobenzoic acid

4-Iodo-3-nitrobenzoic acid synthesis

7synthesis methods

Product Name:4-Iodo-3-nitrobenzoic acid
CAS Number:35674-27-2
Molecular formula:C7H4INO4
Molecular Weight:293.02

1588-83-6
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$6.00/5g

35674-27-2
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$7.00/250mg

Yield:35674-27-2 89.7%

Reaction Conditions:

Stage #1:4-amino-3-nitrobenzoic acid with hydrogenchloride;sodium nitrite in water at 0 - 5; for 1 h;
Stage #2: with potassium iodide in water at 0 - 20; for 2 h;

Steps:

1 Preparation of 4-iodo-3-nitrobenzoic acid (Compound V)
Example 1
Preparation of 4-iodo-3-nitrobenzoic acid (Compound V)
45 g (0.25 mol) 4-Amino-3-nitrobenzoic acid, 400 ml water and 100 ml concentrated hydrochloric acid were added into a reaction flask.
Started to stir, and the mixture was cooled to 0 to 5° C., then 50 ml aqueous solution of 25.9 g sodium nitrite (0.38 mol) was added dropwise.
The solid was dissolved gradually.
After completing the dropwise addition, the mixture was reacted at 0 to 5° C. for 1 hour, and 200 ml aqueous solution of 88 g (0.5 mol) potassium iodide was added dropwise at this temperature.
The mixture was stirred at room temperature for 2 h after completing the dropwise addition, and solid was precipitated.
The solid was filtered, washed with water, and dried to obtain 4-iodo-3-nitrobenzoic acid (compound V) as a solid, 65 g (0.22 mol), yield 89.7%.

References:

Zhejiang Hisun Pharmaceutical Co., Ltd.;Bai, Hua;Zhao, Xuyang;Gong, Yongxiang;Zhong, Jinqing;Zhu, Qifeng;Liu, Xiaoyu;Liu, Lifei;Zhou, Qixian US2013/225810, 2013, A1 Location in patent:Paragraph 0081; 0082

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