Methanesulfonic Acid → Di(6-aminohexyl) 3,3'-thiodipropionate

HRID 1253398Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1253398
CS(O)(=O)=O.[NH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[S:14]([CH2:20][CH2:21][C:22]([OH:24])=O)[CH2:15][CH2:16][C:17]([OH:19])=[O:18]>C(C(C)=O)C(C)C>[S:14]([CH2:15][CH2:16][C:17]([O:19][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])=[O:18])[CH2:20][CH2:21][C:22]([O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])=[O:24]

Komponenten

5

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

8.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 9.4 g of 6-amino-1-hexanol (manufactured by Tokyo Chemical Industry Co., Ltd.). After stirring for 10 minutes, 7.1 g of 3,3′-thiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. and then stirred at 110° C. for 7 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 50 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stirring for 2 hours, the precipitated crystals were collected by filtration and washed with acetone, yielding the methanesulfonate salt of di(6-aminohexyl) 3,3′-thiodipropionate.

Aufarbeitung

  1. stirringstirred at 110° C. for 7 hours
  2. customcompletion of the reaction
  3. temperaturethe reaction mixture was cooled to room temperature
  4. stirringAfter stirring for 2 hours
  5. filtrationthe precipitated crystals were collected by filtration
  6. washwashed with acetone

Quellen und Nachweise

ORD-Eintrag
ord-e1b75d5ab25b4a16bf3f81cf6cb00ff1
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08455413B2

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