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ChemicalBook CAS DataBase List EthanediaMide iMpurity D

EthanediaMide iMpurity D synthesis

3synthesis methods
365998-36-3 Synthesis
tert-butyl (1R,2S,5S)-2-aMino-5-(diMethylcarbaMoyl)cyclohexylcarbaMate

365998-36-3
171 suppliers
$7.00/250mg

349125-08-2 Synthesis
N-(5-Chloropyridin-2-yl)oxalaMic acid ethyl ester

349125-08-2
129 suppliers
$236.47/250mg

EthanediaMide  iMpurity D

480452-36-6
76 suppliers
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Yield:480452-36-6 93%

Reaction Conditions:

with sodium acetate in N,N-dimethyl-formamide at 90; for 7 h;Reagent/catalyst;Temperature;Solvent;

Steps:

1-4 Example 2

DMF (120g) was placed in a 500mL reaction flask,Compound A (22.5 g, 0.079 mol, 1.00 eq.) was added successively,Compound B (18.9g, 0.083mol, 1.05eq.) and sodium acetate (9.7g, 0.118mol, 1.50eq.) were heated to 90° C. to react for 7h. Add 240g of water,Incubate the reaction at 85 °C for 1 h,There is solid precipitation,Suction filtration, the filter cake was rinsed with water,Compound I obtained after drying was off-white solid 34.3g,Yield: 93.0%,Purity: 98.9%.

References:

CN113968813,2022,A Location in patent:Paragraph 0038-0049

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