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Sodium Hydroxide → 4-(Dimethylamino)butanethiol hydrochloride

HRID 266873
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 266873
[OH-].[Na+].[ClH:3].Cl.[CH3:5][N:6]([CH3:15])[CH2:7][CH2:8][CH2:9][CH2:10][S:11]C(=N)N>O>[ClH:3].[CH3:5][N:6]([CH3:15])[CH2:7][CH2:8][CH2:9][CH2:10][SH:11]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 11957708SKF 91488 dihydrochloride

Produkt 1

HCID 190315554-(Dimethylamino)butanethiol hydrochlorideAusbeute 60,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel3×

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

A solution of sodium hydroxide (16.4 g) in water (16.5 ml) was added dropwise under nitrogen at 0° C. to a stirred solution of S-[4-(dimethylamino)butyl]-isothiourea dihydrochloride (51 g) in water (60 ml), then the mixture was heated at 95° C. for 2 hours and allowed to cool to ambient temperature. Water (100 ml) was added, and the product was extracted into ether (50 ml), dichloromethane (3×50 ml), and ether (2×50 ml). The combined organic solutions were dried over magnesium sulphate, then the solvents were removed in vacuo. The residue was dissolved in ether and the solution was saturated with hydrogen chloride. The resulting solid was collected by filtration and dried in vacuo at ambient temperature to give 4-(dimethylamino)butanethiol hydrochloride as a white solid (21 g) which was used without further purification.

Aufarbeitung

  1. temperatureto cool to ambient temperature
  2. extractionthe product was extracted into ether (50 ml), dichloromethane (3×50 ml), and ether (2×50 ml)
  3. dry with materialThe combined organic solutions were dried over magnesium sulphate
  4. customthe solvents were removed in vacuo
  5. dissolutionThe residue was dissolved in ether
  6. filtrationThe resulting solid was collected by filtration
  7. customdried in vacuo at ambient temperature

Quellen und Nachweise

ORD-Eintrag
ord-1f64c6af0f0b4255a5feb84bf4e8c6c9
Quelldatensatz
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05652271

Notizen zur Reaktion

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