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131543-46-9
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Yield:131543-46-9 94%

Reaction Conditions:

Stage #1: ethylenediaminewith sodium nitrate at 46; for 3.83333 h;
Stage #2: ethyl crotonatewith tetrakis(triphenylphosphine)platinum at 57; for 3.33333 h;Temperature;

Steps:

3 Example 3

a method for synthesizing an organic intermediate oxalic acid aldehyde,Including the following steps: A: 2 mol of ethylenediamine was added to the reaction vessel, and the temperature was slowly raised.Raise the temperature to 46 °C in 50 min, Add 1.3L of 22% sodium nitrate solution, Control the stirring speed of 220rpm, After reacting for 3 h, 6 mol of a 41% by mass of ethyl crotonate solution was added.Continue to react for 80 minutes; B: Raise the temperature to 57 °C, add 3 mol of tetrakis(triphenylphosphine) platinum powder, Continue the reaction for 120 min, then lower the temperature to 16 °C. Wash 5 times with a 16% potassium chloride solution,Washing 4 times with a 45% methylene chloride solution,Washed 4 times with a 57% dichloroacetonitrile solution. Recrystallization from a solution of 86% in 2-hexanol,The anhydrous sodium sulfate dehydrating agent was dehydrated to obtain 109.04 g of the finished oxalic acid aldehyde, and the yield was 94%.

References:

CN108238862,2018,A Location in patent:Paragraph 0018; 0019; 0022; 0023; 0024-0027