Erlotinib Impurity 22 synthesis

7synthesis methods

Product Name:Erlotinib Impurity 22
CAS Number:950596-59-5
Molecular formula:C16H23N3O4
Molecular Weight:321.37

950596-58-4 Synthesis

2-Amino-4,5-bis(2-methoxyethoxy)benzonitrile

950596-58-4
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4637-24-5 Synthesis

4637-24-5
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950596-59-5
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Yield:950596-59-5 88%

Reaction Conditions:

with acetic acid in toluene at 80 - 90;

Steps:

1 Example 1 Preparation of N'-[2-Cyano-4,5-bis(2-methoxyethoxy)phenyl]-N,N-dimethyl-formamidine

2-amino-4,5-bis(2-methoxyethoxy)benzonitrile) 70 g, DMF-DMA (N,N-dimethylformamide dimethyl acetal) 34.5 g, toluene 350 mL, The mixture of glacial acetic acid 4mL, mechanical stirring, heated to 80 ~ 90 °C reaction 3 ~ 4h, the reaction is completed, After concentration under reduced pressure, ethyl acetate (60 mL) was added to the concentrated oil, and methyl tert-butyl ether (100 mL) was added. After the solution is heated and clarified, it is cooled and crystallized, that is, it is stirred at a temperature of 15-20°C for 2 hours. Then at a temperature of 0 ~ 5 °C stirring 1h, suction filtration to obtain a solid at a temperature of 20 ~ 25 °C drying under reduced pressure 4 ~ 5h, The compound of formula II is obtained in 73 g in a yield of 88%.

References:

CN105001166,2018,B Location in patent:Paragraph 0034; 0036

236750-65-5 Synthesis