dimethyl 2-chloropropanedioate

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 25 g of guaiacol and 37 g of dimethyl chloromalonate were added dropwise in succession to a sodium methylate solution from 150 ml of methanol and 4.6 g of sodium. The suspension was stirred at 45° C. for 1 hour with the exclusion of moisture, thereafter the methanol was distilled off. The residue was taken up in 200 ml of toluene and washed with water, 1% sodium hydroxide solution and water until the organic phase was colorless. After drying and evaporating the solvent, the residue was distilled. There were obtained 39.5 g of dimethyl (o-methoxyphenoxy)malonate. B.p. 128° C./7 Pa. the methanol was distilled off washed with water, 1% sodium hydroxide solution and water until the organic phase After drying evaporating the solvent the residue was distilled

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 25 g of guaiacol and 37 g of dimethyl chloromalonate were added dropwise in succession to a sodium methylate solution from 150 ml of methanol and 4.6 g of sodium. The suspension was stirred at 45° C. for 1 hour with the exclusion of moisture, thereafter the methanol was distilled off. The residue was taken up in 200 ml of toluene and washed with water, 1% sodium hydroxide solution and water until the organic phase was colorless. After drying and evaporating the solvent, the residue was distilled. There were obtained 39.5 g of dimethyl (o-methoxyphenoxy)malonate. B.p. 128° C./7 Pa. the methanol was distilled off washed with water, 1% sodium hydroxide solution and water until the organic phase After drying evaporating the solvent the residue was distilled

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 1 g of KOH was added to a solution of 2.2 ml of 2-methoxythiophenol in 30 ml of ethanol. The reaction mixture was treated at room temperature with a solution of dimethyl chloromalonate in 5 ml of ethanol, stirred for 1 hour and evaporated. The residue was partitioned between ether and water. The organic phase was dried, concentrated and the residue was purified over silica gel with methylene chloride. 3.6 g of dimethyl (2-methoxy-phenylsulphanyl)malonate, MS: M=270, were obtained. evaporated The residue was partitioned between ether and water The organic phase was dried concentrated the residue was purified over silica gel with methylene chloride

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-Methoxy-phenol (guaiacol) (48 ml) was slowly added to a stirred suspension of potassium carbonate (70.8 g) in acetone (480 ml) followed by heating to 45° C. Then, dimethylchloromalonate (63.2 ml) in acetone (50 ml) was added within 20 min. The reaction mixture was heated to reflux for 16 h. The solvent was evaporated under reduced pressure, the residue taken into water and extracted with DCM. The combined organic layers were dried over sodium sulfate and evaporated. The oily product was crystallized from tert.-butyl-methyl-ether. Dimethyl-(o-methoxyphenoxy)malonate (86 g) was obtained. The reaction mixture was heated to reflux for 16 h The solvent was evaporated under reduced pressure extracted with DCM The combined organic layers were dried over sodium sulfate evaporated The oily product was crystallized from tert.-butyl-methyl-ether

反応条件: temp:40.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of 3-methoxyphenol (115 g) in acetone (1000 ml) was added K2CO3 (115 g). The suspension was stirred at 40° C. for 15 min. A solution of dimethylchloromalonate (133 ml) in acetone was added over a period of 45 min. The resulting brown suspension was stirred overnight at 70° C. Finally, the solvent was removed under reduced pressure and the residue was taken up in water (1000 ml) and extracted twice with DCM (500 ml). The combined organic layers were washed with water (500 ml), dried over Na2SO4, and evaporated to give crude dimethyl-(3-methoxyphenoxy)malonate (230 g) as an orange oil. The product was not purified any further. The resulting brown suspension was stirred overnight at 70° C Finally, the solvent was removed under reduced pressure extracted twice with DCM (500 ml) The combined organic layers were washed with water (500 ml) dried over Na2SO4 evaporated

反応条件: temp:45.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 2-methoxy-phenol (guaiacol) (48 ml) was slowly added to a stirred suspension of potassium carbonate (70.8 g) in acetone (480 ml) followed by heating to 45° C. Then dimethylchloromalonate (63.2 ml) in acetone (50 ml) was added within 20 min. The reaction mixture was heated to reflux for 16 h. The solvent was evaporated under reduced pressure, the residue taken into water and extracted with DCM. The combined organic layers were dried over sodium sulfate and evaporated. The oily product was crystallized from methyl-tert.-butyl-ether to give dimethyl-(2-methoxyphenoxy)malonate (86 g). The reaction mixture was heated to reflux for 16 h The solvent was evaporated under reduced pressure extracted with DCM The combined organic layers were dried over sodium sulfate evaporated The oily product was crystallized from methyl-tert.-butyl-ether