ethyl methyl carbonate

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

実験手順: A mixed solvent of ethylene carbonate and methyl ethyl carbonate was prepared at a capacity ratio of 10:30. To the mixed solvent, 2% by weight of vinylene carbonate, 2% by weight of vinylethylene carbonate, 5% by weight of fluorobenzene, and 5% by weight of phosphazene were added, obtaining a mixed solution. LiPF6 was dissolved in this mixed solution at a concentration of 1.5 mol/L, obtaining a non-aqueous electrolyte. obtaining a mixed solution obtaining a non-aqueous electrolyte

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

実験手順: A mixed solvent of ethylene carbonate and methyl ethyl carbonate was prepared at a capacity ratio of 10:30. To the mixed solvent, 2% by weight of vinylene carbonate, 2% by weight of vinylethylene carbonate, 5% by weight of fluorobenzene, and 5% by weight of phosphazene were added, obtaining a mixed solution. LiPF6 was dissolved in this mixed solution at a concentration of 1.5 mol/L, obtaining a non-aqueous electrolyte. obtaining a mixed solution obtaining a non-aqueous electrolyte

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

実験手順: A 100 ml two-necked reaction flask is dried under vacuum and baked by fire and then cooled by nitrogen gas flow. 50 ml of anhydrous tetrahydrofuran and 1-Methylimidazole (10 mmol, 0.8 ml) are added. n-Butyl lithium agent (12 mmol, 4.8 ml) is slowly added at −78° C. After the reaction has been taken place for 15 minutes, ethyl methyl carbonate (12 mmol, 1.25 g) is added into the flask to react at the room temperature. Extraction with ether and water is carried out and the organic layer is concentrated to obtain a liquid product. The yield is 95%. The obtained product is then reacted with N,N-Dimethylformamide dimethyl acetal (14.25 mmol, 1.89 ml) without any solvent at 100° C. for 10 hrs. Extraction with methylene chloride and water is carried out and the organic layer is concentrated to obtain solids. The yield is 93%. The obtained product is dissolved in ethanol and then added with hydrazine (33.13 mmol, 1.61 ml). The reaction is carried out for 3 hrs at 90° C. The reaction solution is concentrated and extracted by methylene chloride and water. The organic layer is concentrated and separated by n-hexane and ethyl acetate through chromatographic column. The product 4mimp is thus obtained and the yield is 68%. 1H NMR (400 MHz, CD2Cl2): δ 7.44 (d, 1 H, J=0.8 Hz), 7.05 (d, 1 H, J=1.2 Hz), 6.95 (d, 1 H, J=1.2 Hz), 3.87 (s, 3 H), 2.29 (d, J=0.8 z, 3H). A 100 ml two-necked reaction flask is dried under vacuum and baked by fire cooled by nitrogen gas flow for 15 minutes to react at the room temperature Extraction with ether and water the organic layer is concentrated to obtain a liquid product Extraction with methylene chloride and water the organic layer is concentrated to obtain solids The reaction solution is concentrated extracted by methylene chloride and water The organic layer is concentrated separated by n-hexane and ethyl acetate through chromatographic column The product 4mimp is thus obtained

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

実験手順: A 100 ml two-necked reaction flask is dried under vacuum and baked by fire and then cooled by nitrogen gas flow. 50 ml of anhydrous tetrahydrofuran and 1-Methylimidazole (10 mmol, 0.8 ml) are added. n-Butyl lithium agent (12 mmol, 4.8 ml) is slowly added at −78° C. After the reaction has been taken place for 15 minutes, ethyl methyl carbonate (12 mmol, 1.25 g) is added into the flask to react at the room temperature. Extraction with ether and water is carried out and the organic layer is concentrated to obtain a liquid product. The yield is 95%. The obtained product is then reacted with N,N-Dimethylformamide dimethyl acetal (14.25 mmol, 1.89 ml) without any solvent at 100° C. for 10 hrs. Extraction with methylene chloride and water is carried out and the organic layer is concentrated to obtain solids. The yield is 93%. The obtained product is dissolved in ethanol and then added with hydrazine (33.13 mmol, 1.61 ml). The reaction is carried out for 3 hrs at 90° C. The reaction solution is concentrated and extracted by methylene chloride and water. The organic layer is concentrated and separated by n-hexane and ethyl acetate through chromatographic column. The product 4mimp is thus obtained and the yield is 68%. 1H NMR (400 MHz, CD2Cl2): δ 7.44 (d, 1 H, J=0.8 Hz), 7.05 (d, 1 H, J=1.2 Hz), 6.95 (d, 1 H, J=1.2 Hz), 3.87 (s, 3 H), 2.29 (d, J=0.8 z, 3H). A 100 ml two-necked reaction flask is dried under vacuum and baked by fire cooled by nitrogen gas flow for 15 minutes to react at the room temperature Extraction with ether and water the organic layer is concentrated to obtain a liquid product Extraction with methylene chloride and water the organic layer is concentrated to obtain solids The reaction solution is concentrated extracted by methylene chloride and water The organic layer is concentrated separated by n-hexane and ethyl acetate through chromatographic column The product 4mimp is thus obtained

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

実験手順: A mixed solvent of ethylene carbonate and methyl ethyl carbonate was prepared at a capacity ratio of 10:30. To the mixed solvent, 2% by weight of vinylene carbonate, 2% by weight of vinylethylene carbonate, 5% by weight of fluorobenzene, and 5% by weight of phosphazene were added, obtaining a mixed solution. LiPF6 was dissolved in this mixed solution at a concentration of 1.5 mol/L, obtaining a non-aqueous electrolyte. obtaining a mixed solution obtaining a non-aqueous electrolyte

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

実験手順: A 100 ml two-necked reaction flask is dried under vacuum and baked by fire and then cooled by nitrogen gas flow. 50 ml of anhydrous tetrahydrofuran and 1-Methylimidazole (10 mmol, 0.8 ml) are added. n-Butyl lithium agent (12 mmol, 4.8 ml) is slowly added at −78° C. After the reaction has been taken place for 15 minutes, ethyl methyl carbonate (12 mmol, 1.25 g) is added into the flask to react at the room temperature. Extraction with ether and water is carried out and the organic layer is concentrated to obtain a liquid product. The yield is 95%. The obtained product is then reacted with N,N-Dimethylformamide dimethyl acetal (14.25 mmol, 1.89 ml) without any solvent at 100° C. for 10 hrs. Extraction with methylene chloride and water is carried out and the organic layer is concentrated to obtain solids. The yield is 93%. The obtained product is dissolved in ethanol and then added with hydrazine (33.13 mmol, 1.61 ml). The reaction is carried out for 3 hrs at 90° C. The reaction solution is concentrated and extracted by methylene chloride and water. The organic layer is concentrated and separated by n-hexane and ethyl acetate through chromatographic column. The product 4mimp is thus obtained and the yield is 68%. 1H NMR (400 MHz, CD2Cl2): δ 7.44 (d, 1 H, J=0.8 Hz), 7.05 (d, 1 H, J=1.2 Hz), 6.95 (d, 1 H, J=1.2 Hz), 3.87 (s, 3 H), 2.29 (d, J=0.8 z, 3H). A 100 ml two-necked reaction flask is dried under vacuum and baked by fire cooled by nitrogen gas flow for 15 minutes to react at the room temperature Extraction with ether and water the organic layer is concentrated to obtain a liquid product Extraction with methylene chloride and water the organic layer is concentrated to obtain solids The reaction solution is concentrated extracted by methylene chloride and water The organic layer is concentrated separated by n-hexane and ethyl acetate through chromatographic column The product 4mimp is thus obtained