Isostearyl Alcohol EX → HCID 89388392, Verbindung

HRID 511887

Reaktionsgleichung

Reaktionsgleichung von HRID 511887
[CH2:1]([O:19][S:20]([O-:23])(=[O:22])=[O:21])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH:16]([CH3:18])[CH3:17].[Na+:24].[CH2:25]([OH:43])CCCCCCCCCCCCCCC(C)C>>[CH2:1]([O:19][S:20]([O-:23])(=[O:22])=[O:21])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH:16]([CH3:17])[CH3:18].[Na+:24].[C:25](=[O:43])=[O:19]

Komponenten

3

Edukt 2

HCID 62825Isostearyl Alcohol EXHCID 23698004HCID 23698004, Verbindung

Produkt 1

HCID 89388392HCID 89388392, Verbindung

Versuchsvorschrift

Into a piston front part (window side) in the variable-volume high-pressure cell, 0.143 g (0.386 mmol) of sodium isostearylsulfate (containing 13.9% of isostearyl alcohol as an impurity) obtained in Example 1 was charged and the apparatus was closed tightly, followed by drying the inside of the variable-volume high-pressure cell using a vacuum pump. Next, the temperature inside of the variable-volume high-pressure cell was set at 35° C. and into the piston front part of the variable-volume high-pressure cell, 20 g (sodium isostearylsulfate concentration (relative to carbon dioxide): 0.08% by mol) of carbon dioxide (manufactured by Nippon Ekitan Corporation; purity: 99.99% or more) was pressed. Then, the temperature inside of the variable-volume high-pressure cell was elevated to 75° C. and the pressure in the piston rear part of the variable-volume high-pressure cell was set to 37 MPa, followed by stirring the mixture in the variable-volume high-pressure cell to obtain a transparent and homogeneous sodium isostearylsulfate/carbon dioxide solution. Next, to the sodium isostearylsulfate/carbon dioxide solution, 40 μL of a 0.1% by weight sodium p-toluenesulfonate aqueous solution prepared by a method including: dissolving 0.0392 g of p-toluenesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) in 40 mL of water and neutralizing the resultant solution with sodium hydrogen carbonate (manufactured by Wako Pure Chemical Industries, Ltd.); utilizing a six-ports valve and a high pressure pump, was added as the marker solution and the resultant mixture was stirred. At the time when a homogeneous one liquid phase was obtained, an UV-Vis absorption spectrum was measured by a spectrophotometer (manufactured by Hitachi High-Technologies Corporation; U-2810) through a pressure resistant spectrum cell (manufactured by L. TEX Corporation; light path length: 10 mm) having a quartz window that was connected to the apparatus. By repeating the addition of 40 μL of a sodium p-toluenesulfonate aqueous solution, the stirring of the reaction mixture, and the measurement of the UV-Vis absorption spectrum, the data until W0=86.5 (W0c=71.5) were collected.

Aufarbeitung

  1. customobtained in Example 1
  2. additionwas charged
  3. customthe apparatus was closed tightly
  4. customby drying the inside of the variable-volume high-pressure cell
  5. customwas set at 35° C. and into the piston front part of the variable-volume high-pressure cell, 20 g (sodium isostearylsulfate concentration (relative to carbon dioxide): 0.08% by mol) of carbon dioxide (manufactured by Nippon Ekitan Corporation; purity: 99.99% or more)
  6. customwas elevated to 75° C.

Quellen und Nachweise

ORD-Eintrag
ord-35ad1a02c7674ba6a0904991a7a22658
Quelldatensatz
uspto-grants-2015_08
Patentnummer
US09101894B2

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