dimethyl 2-formylbutanedioate

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 60 g of paraformaldehyde are added to a solution of 6.0 g of acetic acid and 6.75 g of dimethylamine in 800 g of methanol, after which 348 g of dimethyl 2-formylsuccinate are added dropwise in the course of 20 minutes. The mixture is stirred for 7 hours at 50° C. and allowed to cool, and methanol and methyl formate are distilled off. The residue is taken up in ethyl acetate and the solution is washed with 100 g of 10% strength sulfuric acid and distilled. 305 g of isomer-free dimethyl itaconate of boiling point 42°-43° C. under 0.3-0.4 mbar are obtained, corresponding to a yield of 96.4% of theory. to cool methanol and methyl formate are distilled off the solution is washed with 100 g of 10% strength sulfuric acid distilled

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl imidocarbamate (437 mg, 0.861 mmol) and dimethyl 2-formylbutanedioate (450 mg, 2.58 mmol) in NMP (5 mL) was added K2CO3 (357 mg, 2.58 mmol). The mixture was heated at 130° C. for 1.5 h. Purification via reverse phase flash chromatography then afforded the title compound, together with ethyl ester (102 mg, 0.211 mmol, 24.55% yield). Purification via reverse phase flash chromatography

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl imidocarbamate (437 mg, 0.861 mmol) and dimethyl 2-formylbutanedioate (450 mg, 2.58 mmol) in NMP (5 mL) was added K2CO3 (357 mg, 2.58 mmol). The mixture was heated at 130° C. for 1.5 h. Purification via reverse phase flash chromatography then afforded the title compound, together with ethyl ester (102 mg, 0.211 mmol, 24.55% yield). Purification via reverse phase flash chromatography

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 60 g of paraformaldehyde are added to a solution of 6.0 g of acetic acid and 6.75 g of dimethylamine in 800 g of methanol, after which 348 g of dimethyl 2-formylsuccinate are added dropwise in the course of 20 minutes. The mixture is stirred for 7 hours at 50° C. and allowed to cool, and methanol and methyl formate are distilled off. The residue is taken up in ethyl acetate and the solution is washed with 100 g of 10% strength sulfuric acid and distilled. 305 g of isomer-free dimethyl itaconate of boiling point 42°-43° C. under 0.3-0.4 mbar are obtained, corresponding to a yield of 96.4% of theory. to cool methanol and methyl formate are distilled off the solution is washed with 100 g of 10% strength sulfuric acid distilled

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl imidocarbamate (437 mg, 0.861 mmol) and dimethyl 2-formylbutanedioate (450 mg, 2.58 mmol) in NMP (5 mL) was added K2CO3 (357 mg, 2.58 mmol). The mixture was heated at 130° C. for 1.5 h. Purification via reverse phase flash chromatography then afforded the title compound, together with ethyl ester (102 mg, 0.211 mmol, 24.55% yield). Purification via reverse phase flash chromatography

反应条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 2-(4-{[4-chloro-3-(trifluoromethyl)phenyl]oxy}phenyl)ethyl imidocarbamate (437 mg, 0.861 mmol) and dimethyl 2-formylbutanedioate (450 mg, 2.58 mmol) in NMP (5 mL) was added K2CO3 (357 mg, 2.58 mmol). The mixture was heated at 130° C. for 1.5 h. Purification via reverse phase flash chromatography then afforded the title compound, together with ethyl ester (102 mg, 0.211 mmol, 24.55% yield). Purification via reverse phase flash chromatography

反应条件: temp:50.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 60 g of paraformaldehyde are added to a solution of 6.0 g of acetic acid and 6.75 g of dimethylamine in 800 g of methanol, after which 348 g of dimethyl 2-formylsuccinate are added dropwise in the course of 20 minutes. The mixture is stirred for 7 hours at 50° C. and allowed to cool, and methanol and methyl formate are distilled off. The residue is taken up in ethyl acetate and the solution is washed with 100 g of 10% strength sulfuric acid and distilled. 305 g of isomer-free dimethyl itaconate of boiling point 42°-43° C. under 0.3-0.4 mbar are obtained, corresponding to a yield of 96.4% of theory. to cool methanol and methyl formate are distilled off the solution is washed with 100 g of 10% strength sulfuric acid distilled