Methanesulfonic Acid → HCID 59584818, Verbindung

HRID 1253402

Reaktionsgleichung

Reaktionsgleichung von HRID 1253402
CS(O)(=O)=O.[NH2:6][CH:7]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:8][OH:9].[C:14]([OH:25])(=O)[CH2:15][CH2:16][S:17][S:18][CH2:19][CH2:20][C:21]([OH:23])=[O:22]>C(C(C)=O)C(C)C>[C:21]([O:23][CH2:8][CH:7]([NH2:6])[CH2:10][CH2:11][CH2:12][CH3:13])(=[O:22])[CH2:20][CH2:19][S:18][S:17][CH2:16][CH2:15][C:14]([O:9][CH2:8][CH:7]([NH2:6])[CH2:10][CH2:11][CH2:12][CH3:13])=[O:25]

Komponenten

5

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

6.1 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 7.0 g of 2-amino-1-hexanol (manufactured by Aldrich Co., Ltd.). After stifling for 10 minutes, 6.3 g of 3,3′-dithiodipropionic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added, and the resulting mixture was heated to 120° C. The mixture was then stirred at 120 to 129° C. for a further 3 hours. Following completion of the reaction, the reaction mixture was cooled to room temperature and then added gradually to 100 mL of methyl isobutyl ketone (manufactured by Wako Pure Chemical Industries, Ltd.). After stifling for 1 hour, the precipitated crystals were collected by filtration and dried at 50° C., yielding the methanesulfonate salt of di(2-aminohexyl) 3,3′-dithiodipropionate.

Aufarbeitung

  1. customcompletion of the reaction
  2. temperaturethe reaction mixture was cooled to room temperature
  3. waitAfter stifling for 1 hour
  4. filtrationthe precipitated crystals were collected by filtration
  5. customdried at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-1477f1b097fe4093b22526e1171ef0a6
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08455413B2

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