Reaktion #4018

Reaktionsgleichung

2-amino-4-trifluoromethylthiophenol hydrochloride

2-chloro-1,1,1-triethoxyethane

→

2-Chloromethyl-5-trifluoromethylbenzothiazole

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   EinengenThe solution was concentrated
2. 2
   Sonstigeto remove excess ethanol
3. 3
   Extraktionthe resulting material was extracted with ether (500 ml)
4. 4
   ExtraktionThe organic extract
5. 5
   Waschenwas washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml)
6. 6
   Sonstigeevaporated
7. 7
   Sonstigeto obtain an amber colored oil, which
8. 8
   Sonstigecrystallized
9. 9
   Sonstigeupon standing at room temperature

Vorschrift

To a solution of 2-amino-4-trifluoromethylthiophenol hydrochloride (30.0 g) in ethanol (125 ml) was added 2-chloro-1,1,1-triethoxyethane (31.0 g). The mixture was heated for 1 hour at 60° C. The solution was concentrated to remove excess ethanol and the resulting material was extracted with ether (500 ml). The organic extract was washed successively with 10% HCl (20 ml), water (100 ml), 10% sodium bicarbonate solution and water (100 ml), and then evaporated to obtain an amber colored oil, which crystallized upon standing at room temperature (28.9 g; m.p. 52° C).

Quelle