반응 #1747833

반응 방정식

N-methylpyrrolidine

chloromethyl methyl ether

→

N-methoxymethyl-N-methylpyrrolidinium chloride

용매

methyl acetate

반응 조건

후처리

1. 1
   온도the temperature was slowly raised
2. 2
   workup.STIRRINGthe mixture was stirred at room temperature for 10 hours
3. 3
   기타the reaction
4. 4
   여과The reaction mixture was filtered
5. 5
   세척the solid product was washed with 150 g of methyl acetate and 150 g of acetone
6. 6
   기타The washed product was dried in a vacuum

실험 절차

A 30.0 g quantity of N-methylpyrrolidine (reagent, product of Tokyo Kasei Co., Ltd.) was dissolved in 120 g of methyl acetate, followed by replacement with nitrogen. A 31.2 g quantity of chloromethyl methyl ether (reagent, product of Tokyo Kasei Co., Ltd.) was added dropwise to the solution at 5° C. over a period of 1 hour. The mixture was stirred at 5° C. for 1 hour, the temperature was slowly raised, and the mixture was stirred at room temperature for 10 hours to complete the reaction. The reaction mixture was filtered, and the solid product was washed with 150 g of methyl acetate and 150 g of acetone. The washed product was dried in a vacuum, giving 53.7 g of N-methoxymethyl-N-methylpyrrolidinium chloride. The chloride salt (53.7 g) obtained was dissolved in 125 g of methanol, and 99.6 g of 30% HBF4 methanol solution was added to the solution. Nitrogen was bubbled through the mixture at 130° C. to remove methanol, hydrogen chloride and excessive HBF4 to obtain 70.2 g of the desired electrolyte, i.e., N-methoxymethyl-N-methylpyrrolidinium tetrafluoroborate (water content: 20 ppm). The electrolyte was used to prepare 100 g of an electrolytic solution of the following composition within a glove box having an argon atmosphere with a dew point of −60° C. Calcium oxide (1.0 g) was thereafter added to the solution.

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