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

HRID 1253399

Reaktionsgleichung

Reaktionsgleichung von HRID 1253399
CS(O)(=O)=O.[NH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[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][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])(=[O:22])[CH2:20][CH2:19][S:18][S:17][CH2:16][CH2:15][C:14]([O:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][NH2:6])=[O:25]

Komponenten

5

Edukt 3

HCID 6395Methanesulfonic AcidHCID 199606-Amino-1-hexanolHCID 951163,3'-Dithiodipropionic acid

Produkt 1

HCID 59584809Di(6-aminohexyl) 3,3'-dithiodipropionate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7909Methyl Isobutyl KetoneLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

2.0 g of methanesulfonic acid (manufactured by Wako Pure Chemical Industries, Ltd.) was added dropwise, under an atmosphere of nitrogen and at 70° C., to 2.3 g of 6-amino-1-hexanol (manufactured by Tokyo Chemical Industry Co., Ltd.). After stirring for 10 minutes, 2.1 g of 3,3′-dithiodipropionic 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 3 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 vacuum filtration and washed with acetone, yielding the methanesulfonate salt of di(6-aminohexyl) 3,3′-dithiodipropionate.

Aufarbeitung

  1. stirringstirred at 110° C. for 3 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 vacuum filtration
  6. washwashed with acetone

Quellen und Nachweise

ORD-Eintrag
ord-5032cbba7aaf45d4a4653b80204863c5
Quelldatensatz
uspto-grants-2013_06
Patentnummer
US08455413B2

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