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22316-45-6

ethyl 3-[(5-chloro-2-nitrophenyl)phenylamino]-3-oxopropionate synthesis

4synthesis methods
25781-92-4 Synthesis
5-CHLORO-2-NITRODIPHENYLAMINE

25781-92-4
196 suppliers
$15.00/1g

36239-09-5 Synthesis
Ethyl malonyl chloride

36239-09-5
281 suppliers
$12.00/5g

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Yield:22316-45-6 91%

Reaction Conditions:

in acetonitrile; for 12 h;Reflux;Large scale;

Steps:

1 Preparation of Compound II

In a 20 L reaction flask,2.5 kg of 2-nitro-5-chlorodiphenylamine was added,16L anhydrous acetonitrile,1.8 kg of malonic acid monoethyl ester chloride,The reaction was heated to reflux for 12 hours.60 vacuum distillation in addition to acetonitrile,Add 8L ethanol stirring dissolved,0 ~ 5 cooling crystallization, pumping filter, dried at 60 yellow crystal weight 3.3kg.Melting point 85-87 ° C, yield 91%.

References:

CN106749052,2017,A Location in patent:Paragraph 0027; 0028