ChemicalBook CAS DataBase List 3-Nitrosalicylic acid

3-Nitrosalicylic acid synthesis

11synthesis methods

Product Name:3-Nitrosalicylic acid
CAS Number:85-38-1
Molecular formula:C7H5NO5
Molecular Weight:183.12

69-72-7 Synthesis

69-72-7
1221 suppliers
$5.00/10g

85-38-1
249 suppliers
$12.00/1g

Yield:85-38-1 99.8%

Reaction Conditions:

with iron(III) hexacyanoferrate(II);nitric acid;acetic acid at 50;Flow reactor;regioselective reaction;Reagent/catalyst;

Steps:

1.1; 1.2; 1.3; 1.4-5.1; 5.2; 5.3; 5.4; 5.5; 1.1; 1.2; 1.3; 1.4; 1.5
1) Measure 900mL of 99% acetic acid, 2.5g of Prussian blue, and 100g of salicylic acid into 2L beaker A to obtain material 1. Weigh 104.4g of concentrated nitric acid with a mass fraction of 65% and pour into 200mL beaker B to obtain Material 2.2) Connect beaker A and beaker B to metering pump P1 and metering pump P2; start metering pump P1 first, feed material 1 to the preheating module, and preheat at 50°C for 1 minute.3) Then start the metering pump P2, and feed the material 2 and the preheated material 1 to the mixing module at the same time. After the mixing module is evenly mixed, material 3 is obtained; the mixing module is set to a temperature of 50°C,The mixing time is 1 minute.4) Feed the material 3 to the reaction module to continue the reaction, and the material 4 is obtained after the reaction is completed.The temperature of the reaction module is set to 50°C, and the reaction time is 1 minute.5) Then the material 4 is poured into the collection module containing 4L of ice water, the temperature in the collection module is maintained at 0°C, and the mixture is stirred for 1 hour.After the stirring is completed, filter the system in the collection module, take the solid and dry,The final product was obtained, weighing 131g, and the total yield was 99.8%. The content of the final product was determined by high performance liquid phase.The purity of 3-nitrosalicylic acid is 99.8%, and the purity of 5-nitrosalicylic acid is 0.2%.

References:

CN112538018, 2021, A Location in patent:Paragraph 0047-0087

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321-14-2 Synthesis