ChemicalBook CAS DataBase List 5-Chloropyridine-2-carboxylic acid

5-Chloropyridine-2-carboxylic acid synthesis

10synthesis methods

Product Name:5-Chloropyridine-2-carboxylic acid
CAS Number:86873-60-1
Molecular formula:C6H4ClNO2
Molecular Weight:157.55

89809-64-3 Synthesis

89809-64-3
256 suppliers
$14.00/5g

86873-60-1
241 suppliers
$7.00/1g

Yield:86873-60-1 81.4%

Reaction Conditions:

with water;sodium hydroxide in ethanol at 90 - 100; for 1.5 h;

Steps:

1.5 5) Preparation of Intermediate 5
1000ml four-necked flask, fitted with a stirrer, thermometer, reflux condenser, is added 5-chloro-2-cyano-pyridine (27.7g, 0.2mo), 277 mg of the ethanol, and dissolved with stirring, an aqueous solution of 10% NaOH was added 277ml, heated to 90 ~ 100 stirred at reflux for 1.5h, TLC TLC [discriminating the end of reaction conditions to expand (butanol - acetic acid - water = 5: 2: 2)], the reaction is complete, cooled to room temperature under stirring, the pH was adjusted to 2 with 2NHCl ~ 3, and concentrated under reduced pressure to a volume of 100ml, methanol was added to 200ml, cooled to 0 ~ 5 , filtered, the solid out, and the filtrate was concentrated to dryness under reduced pressure, the residue was added 450ml of dichloromethane and 50ml of methanol, stirred for 1h, filtered and the solid with the amount of 10% methanol - methylene chloride mixture was washed, 60 ~ 65 vacuum oven vacuum drying 2h, as a white solid intermediate 525.5g, a yield of 81.4%.

References:

Anhui Yi Xin Ming Pharmaceutical Co., Ltd.;Xu, Hui;Tao, Junyu CN105348187, 2016, A Location in patent:Paragraph 0014; 0032

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40473-01-6 Synthesis