N-Methylpiperidine → 1-Methyl-3-propyl piperidinium propyl sulfate

HRID 1821108노트

반응식

HRID 1821108 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.[CH2:8]([O:11][S:12](=[O:18])(=[O:17])[O:13][CH2:14][CH2:15][CH3:16])[CH2:9][CH3:10]>C1(C)C=CC=CC=1>[CH2:8]([O:11][S:12]([O-:18])(=[O:17])=[O:13])[CH2:9][CH3:10].[CH3:1][NH+:2]1[CH2:7][CH2:6][CH2:5][CH:4]([CH2:14][CH2:15][CH3:16])[CH2:3]1

참가 물질

4

반응물 2

HCID 12291N-MethylpiperidineHCID 69015Sulfuric acid, dipropyl ester

생성물 1

HCID 866083801-Methyl-3-propyl piperidinium propyl sulfate수율 95%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

To a 50 ml four necked flask equipped with a stirrer, a dropping funnel, a cooling tube and a thermometer, 4.96 g (0.05 mol) of 1-methyl piperidine and 5 ml of toluene were charged, after heating to 50° C., 10.02 g (0.055 mol) of dipropyl sulfuric acid was dropped slowly taking one hour or more. After reacting for 10 hours, 13.37 g of 1-methyl-3-propyl piperidinium propyl sulfate was obtained by drying under a reduced pressure. Then, 13.37 g of the obtained 1-methyl-3-propyl piperidinium propyl sulfate was dissolved in 8 ml of water, and a solution in which 10.5 g of potassium bis(fluorosulfonyl)imide was dissolved in 8 ml of water was added thereto at a room temperature and stirred. From separated two layers, the lower layer was fractionated and by-products were removed by adding 40 wt % of purified water and water washing five times, and vacuum drying was applied to obtain 15.31 g of 1-methyl-3-propyl pyrrolinium bis(fluorosulfonyl) imide. As a result of ICP analysis, the total alkali metals was 1.8 ppm, chloride ion was 0.5 ppm, and each of iodide and bromide ions was 0.1 ppm or less (lower than ICP detection limit).

후처리

  1. waittaking one hour or more

출처 및 근거

ORD 기록
ord-ec81efdcf14f48acbec3bde5431e329b
출처 데이터셋
uspto-grants-2009_10
특허 번호
US07605271B2

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