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1-Octanol → HCID 178443872, 화합물

HRID 1441914
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HRID 1441914 반응식
[S:1]([O:6]C)([O:4][CH3:5])(=[O:3])=[O:2].C([C:12]1[NH:13][CH:14]=[CH:15][N:16]=1)CCC.[CH2:17](O)[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]>CO>[CH2:5]([O:4][S:1]([O-:6])(=[O:3])=[O:2])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23].[CH2:21]([N+:16]1[CH:15]=[CH:14][N:13]([CH3:5])[CH:12]=1)[CH2:22][CH2:23][CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 9571-OctanolHCID 6497Dimethyl SulfateHCID 118153512-butyl-1H-imidazole

생성물 1

HCID 178443872HCID 178443872, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a 250 ml Schlenk flask, 48.04 g (0.381 moles) of dimethyl sulfate was slowly added dropwise to 47.31 g (0.381 moles) of butylimidazole with ice cooling and under a blanket gas. Stirring of the mixture was continued at room temperature over night. After the addition of 62.72 g (0.482 moles; 1.26 equ.) of 1-octanol and 0.67 g of Dowex ion-exchanger washed with acetone and dried under high vacuum, the mixture was allowed to react over night at 140° C., and at the same time, the by-product methanol formed was removed from the reaction mixture by sparging with an argon stream. The remaining volatile fractions were subsequently removed under high vacuum at 80° C. The product, 1-butyl-3-methylimidazolium 1-octyl sulfate, was obtained as a viscous, slightly yellow liquid in quantitative yield. The product does not contain any detectable amounts of Cl− contamination (AgNO3 test; <3 ppm).

후처리

  1. waitwas continued at room temperature over night
  2. washwashed with acetone
  3. customdried under high vacuum
  4. customto react over night at 140° C.
  5. customwas removed from the reaction mixture
  6. customby sparging with an argon stream
  7. customThe remaining volatile fractions were subsequently removed under high vacuum at 80° C

출처 및 근거

ORD 기록
ord-218402e4a71a463f810bb19150e54d1a
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07655803B2

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