Toluene → N-methyl-N-propylpyrrolidinium ethylsulfamate

HRID 2075294

反応式

HRID 2075294 の反応式
[CH3:1][N:2]1[CH2:6][CH2:5][CH2:4][C:3]1=O.[S:8]([O:13]CC)([O:10]CC)=[O:9].[C:16]1(C)[CH:21]=CC=C[CH:17]=1>>[CH2:3]([NH:2][S:8](=[O:10])(=[O:9])[O-:13])[CH3:4].[CH3:1][N+:2]1([CH2:17][CH2:16][CH3:21])[CH2:6][CH2:5][CH2:4][CH2:3]1

参加物

4

反応物 3

HCID 1140TolueneHCID 12197Sulfurous acid, diethyl esterHCID 13387N-methyl-2-pyrrolidone

生成物 1

HCID 67091120N-methyl-N-propylpyrrolidinium ethylsulfamate

実験手順

200 mmol of 1-methylpyrrolidone (Aldrich) in solution in 100 ml of toluene were quaternized with 100 mmol of diethyl sulfite (Aldrich), added slowly at 0° C., with stirring for 24 hours at ambient temperature. After evaporation of the solvent and drying, N-methyl-N-propylpyrrolidinium ethylsulfamate was obtained. 50 mmol of ethylsulfamate were solubilized in 50 ml of acetonitrile, and were reacted with 50 mmol of KBFFST. After stirring for 2 hours, and then filtration, evaporation of the solvent and drying, the N-propane-N-methylpyrrolidinium salt of 3,5-difluorosulfonyl-1,2,4-triazole (PYR13BFST) corresponding to the following formula was obtained:

後処理

  1. additionadded slowly at 0° C.
  2. customAfter evaporation of the solvent
  3. customdrying

出典と根拠

ORDレコード
ord-50e4c088b3ce4d6f9f063c0172bf41d2
出典データセット
uspto-grants-2011_04
特許番号
US07919629B2

関連ノート

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