2-(dimethoxymethyl)quinoxaline 1,4-dioxide synthesis
- Product Name:2-(dimethoxymethyl)quinoxaline 1,4-dioxide
- CAS Number:32065-66-0
- Molecular formula:C11H12N2O4
- Molecular Weight:236.22
Yield:32065-66-0 46.6%
Reaction Conditions:
with pyrrolidine in dichloromethane at 0; for 5 h;
Steps:
14.1 Step 1: Preparation of 2-(dimethoxymethyl)quinoxaline-1,4-dioxide
Acetaldehyde dimethyl acetal (71 g, 0.6 mol, 1 eq)And tetrahydropyrrole (43 g, 0.6 mol, 1 eq) were dissolved in about 200 ml of DCM,Ice bath to 0 ° C,After benzofuroxan (82g, 0.6mol, 1eq) in DCM over 1 hour with stirring was added dropwise,While maintaining the temperature of the solution at 0 ° C.After completion of the dropwise addition, the reaction was continued for 4 hours under an ice bath,TLC shows that the basic reaction of benzofurazine is complete.Spin dry solvent DCM,Get viscous liquid,Ice bath to cool the product,Add petroleum ether to the reaction flask,There is solid precipitation,Filter with a sand core funnel,The filter cake was washed with ethanol (250 ml * 3)To give a pale yellow solid (2- (dimethoxymethyl) quinoxaline-1,4-dioxide) 66g.Yield: 46.6%.
References:
CN104447587,2017,B Location in patent:Paragraph 0081; 0082; 0083
