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ChemicalBook CAS DataBase List 5-Nitrosalicylic acid
96-97-9

5-Nitrosalicylic acid synthesis

15synthesis methods
-

Yield:96-97-9 89.34%

Reaction Conditions:

with tert.-butylhydroperoxide;potassium tert-butylate;copper(ll) bromide in acetonitrile at 80; for 5 h;Reagent/catalyst;

Steps:

3; 4; 5 Example 3
Add 5-nitrosalicylic aldehyde (16.7g, 0.1mol),Potassium tert-butoxide (22.4g, 0.2mol),Copper bromide(1.1g, 5mmol)And acetonitrile (250ml),70% tert-butyl hydroperoxide (26g, 0.1mol) was added dropwise with stirring,React at 80°C for 5h,After the reaction is over, concentrate under reduced pressure to remove the solvent, pour cold water into the residue, stir, and filter with suction. The filtrate is adjusted to pH 23 with hydrochloric acid, filtered with suction, and dried to obtain a pale yellow solid 5-nitrosalicylic acid ( 13.6g, 89.34%),The purity is 97.31%,The schematic diagram of 1HNMR is shown in Figure 2.

References:

Changzhou Engineering Polytechnic College;Zhang Wenwen;Gong Bingqian;Yang Liping;Weng Zhibing;Ye Aiying;Wang Yupeng CN111533663, 2020, A Location in patent:Paragraph 0011; 0041-0047

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