Methyl Methoxymethylenecyanoacetate synthesis

4synthesis methods

Product Name:Methyl Methoxymethylenecyanoacetate
CAS Number:13974-74-8
Molecular formula:C6H7NO3
Molecular Weight:141.12

67-56-1 Synthesis

67-56-1
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METHYL 2-CYANO-3-(DIMETHYLAMINO)ACRYLATE

1187-27-5
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13974-74-8
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Yield:13974-74-8 97.89 %

Reaction Conditions:

with hydrogenchloride in water at 78;

Steps:

8

with a thermometer,In the reaction flask with reflux condenser and stirring paddle,Add 150mL methanol and the compound (2-cyano-3-(dimethylamino)methyl acrylate) (0.5mol) described in the formula (Ib) that Preparation Example 1 obtains successively,Warm up to 78°C under stirring for slight reflux,Then a saturated methanol solution of hydrogen chloride (4M, 625 mL) was slowly added dropwise,2h dropwise addition is completed,Reflux reaction 3h,After monitoring the reaction,Remove the solvent,And add 500mL dichloroethane and 500mL water to extract,to obtain the organic phase,And wash the organic phase with 500mL of saturated brine,Take the organic phase and desolventize,71.77 g of the compound represented by formula (Ib) (methyl 2-cyano-3-methoxyacrylate) was obtained, with a purity of 96.18 wt % and a yield of 97.89 %.

References:

CN115215767,2022,A Location in patent:Paragraph 0102-0106