ChemicalBook CAS DataBase List 2-Chloro-4-methyl-3-nitropyridine

2-Chloro-4-methyl-3-nitropyridine synthesis

5synthesis methods

Product Name:2-Chloro-4-methyl-3-nitropyridine
CAS Number:23056-39-5
Molecular formula:C6H5ClN2O2
Molecular Weight:172.57

21901-18-8

23056-39-5

General procedure for the synthesis of 2-chloro-4-methyl-3-nitropyridine from 2-keto-3-nitro-4-methylpyridine: 2-keto-3-nitro-4-methylpyridine (13 g, 0.084 mol) was added to 50 mL of phosphorochloridic acid chloride and heated to reflux for 4 hours. Upon completion of the reaction, the excess phosphorus trichloride was removed by distillation. The crude product was recrystallized in 50 mL of 75% ethanol solution to give 11 g of white solid product in 75.3% yield. The melting point of the product was 51.7-52.1 °C (ethanol), which is consistent with the values reported in the literature (52.0-52.9 °C) [J.O.C., 1955, 20, 1729-1731].

21901-18-8 Synthesis

21901-18-8
246 suppliers
$25.00/5g

23056-39-5
341 suppliers
$6.00/1g

Yield:23056-39-5 75.3%

Reaction Conditions:

with trichlorophosphate for 4 h;Reflux;

Steps:

1
Synthesis of the compound 10 The compound 9 (13g, 0.084mol) was added into 50mL of phosphorus oxychloride, the mixture was heated under reflux for 4 h, and distilled to remove excessive phosphorus oxychloride. The resulted product was recrystallized in 50mL of ethanol (75%) to yield 11 g of a white solid product with yield of 75.3%. The melting point: 51.7-52.1 °C(ethanol) (M.P. 52.0-52.9 °C was reported in reference)[J.O.C., 1955, 20, 1729-1731].

References:

Beijing Yiling Bioengineering Co., Ltd. EP2366691, 2011, A1 Location in patent:Page/Page column 7

FullText

21901-18-8 Synthesis

21901-18-8
246 suppliers
$25.00/5g

23056-39-5
341 suppliers
$6.00/1g

References

6635-86-5 Synthesis