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ChemicalBook CAS DataBase List 3-Amino-6-chloro-benzo[b]thiophene-2-carboxylic acid methyl ester
35212-87-4

3-Amino-6-chloro-benzo[b]thiophene-2-carboxylic acid methyl ester synthesis

2synthesis methods
57381-51-8 Synthesis
4-Chloro-2-fluorobenzonitrile

57381-51-8
193 suppliers
$6.00/1g

2365-48-2 Synthesis
Methyl thioglycolate

2365-48-2
367 suppliers
$19.00/25g

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Yield:35212-87-4 92%

Reaction Conditions:

with sodium tertiary butoxide in N,N-dimethyl-formamide at -5 - 20; for 2 h;

Steps:

1 Synthesis of intermediate A-1

To a 3 L round bottom flask were added 4-chloro-2-fluorobenzonitrile (100 g, 0.64 mol) and methyl thioglycolate (70.0 ml, 0.77 mol) add 1.2 L of N, N-dimethylformamide and lower the internal temperature to -5 ° C. Sodium tert-butoxide (93.67 g, 0.96 mol) is slowly added, ensuring that the internal temperature does not exceed 0 ° C. After stirring at room temperature for 2 hours, Drop the reaction slowly into cold water. The resulting solid was stirred at room temperature, filtered, Drying afforded intermediate A-1. (142.9 g, 92%).

References:

KR2019/32884,2019,A Location in patent:Paragraph 0335-0339