2-(Methylamino)ethanol → 2-(Methyl(2-hydroxyethyl)amino)benzothiazole

HRID 441010

Reaktionsgleichung

Reaktionsgleichung von HRID 441010
Cl[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1.[CH3:11][NH:12][CH2:13][CH2:14][OH:15]>O>[CH3:11][N:12]([CH2:13][CH2:14][OH:15])[C:2]1[S:3][C:4]2[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=2[N:6]=1

Komponenten

4

Edukt 2

HCID 80162-(Methylamino)ethanolHCID 119872-Chlorobenzothiazole

Produkt 1

HCID 6008992-(Methyl(2-hydroxyethyl)amino)benzothiazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 2-chlorobenzothiazole (8.5 g) and 2-methylaminoethanol (20 ml) was heated at 120° C. under pressure in a sealed, glass lined, stainless steel reaction vessel for 18 hours. After cooling, the oil was added to water (100 ml), extracted with dichloromethane (2×100 ml), the organic extracts were dried (MgSO4), filtered and evaporated to dryness. Chromatography of the residual oil on silica-gel in 2 1/2% methanol in dichloromethane gave the title compound which was used in Preparation 1 without further purification.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with dichloromethane (2×100 ml)
  3. dry with materialthe organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated to dryness

Quellen und Nachweise

ORD-Eintrag
ord-dd16115d3c764d12ad95e7fc563e0aa1
Quelldatensatz
uspto-grants-1996_05
Patentnummer
US05521201

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