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1,3-Dichloro-2-propanol → 1,3-Bis(2-(dimethylamino)ethylthio)-2-propanol

HRID 581645
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 581645
Cl.[CH3:2][N:3]([CH3:7])[CH2:4][CH2:5][SH:6].[OH-].[Na+].Cl[CH2:11][CH:12]([OH:15])[CH2:13]Cl>C(O)C>[CH3:2][N:3]([CH3:7])[CH2:4][CH2:5][S:6][CH2:11][CH:12]([OH:15])[CH2:13][S:6][CH2:5][CH2:4][N:3]([CH3:7])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 72891,3-Dichloro-2-propanolHCID 14798Sodium HydroxideHCID 25798Captamine Hydrochloride

Produkt 1

HCID 538484991,3-Bis(2-(dimethylamino)ethylthio)-2-propanolAusbeute 85,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

2-(Dimethylamino)ethanethiol hydrochloride (10.78 g, 78 mmole) was added portion-wise to a solution of sodium hydroxide (6.2 g, 155 mmole) in ethanol (40 mL) at 0° C. under nitrogen. A further portion of ethanol (20 mL) was added and the mixture stirred at this temperature for 10 minutes. 1,3-Dichloro-2-propanol (5.29 g, 41 mmole) was added dropwise. On completion of the addition, the reaction mixture was allowed to warm to room temperature and stirred for a further 2 hours. The precipitated solid was filtered off and the washed with ethanol. The filtrate was evaporated. The resulting oil was taken up into acetone, filtered and evaporated to give the desired product (8.90 g, 68%) as a pale yellow oil.

Aufarbeitung

  1. additionOn completion of the addition
  2. stirringstirred for a further 2 hours
  3. filtrationThe precipitated solid was filtered off
  4. washthe washed with ethanol
  5. customThe filtrate was evaporated
  6. filtrationfiltered
  7. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-7f7856a28c464f0c9a0eed16e605b3c2
Quelldatensatz
uspto-grants-1999_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05922527

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