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ChemicalBook CAS DataBase List 6-Methyl-2-pyridinecarboxylic acid
934-60-1

6-Methyl-2-pyridinecarboxylic acid synthesis

13synthesis methods
-

Yield: 75%

Reaction Conditions:

with potassium permanganate in water-d2 at 20 - 60; for 5 h;

Steps:

1.1
Step 1: compound 1 (10.71g, 0 . 1mol) dissolved in 500 ml deionized water, stirred and heated up to 60 °C. Then the 23.7g (0.15mol) the KMnO4 solid-in into the above-mentioned solution for ten times, the time interval between the two times for 30 min. Strict control of temperature in the 60 °C left and right, the reaction at room temperature to 5h. After the reaction is ended immediately used to remove insoluble impurity. PH=5 level to the acidity, then using the ethyl acetate extraction, collecting the organic phase, decompression turns on lathe does, recrystallized with ethanol to obtain compound 2 (10.3g, 75%).In this step of trying to adopt different reaction condition such as KMnO4equivalent are respectively 1,1.5,2, potassium permanganate adopt different PH, temperature, molar compared to passing through orthogonal experiment to obtain the optimal conditions for neutral potassium permanganate aqueous solution, KMnO4to 1.5 equivalent.

References:

Shanghai Institute Of Technology;Yao, Zhiyi;Zhang, Xiaopan;Zong, Haoqiang;Wang, Dongsheng CN105294552, 2016, A Location in patent:Paragraph 0047; 0048; 0049; 0050

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