Reaktion #1859510

Reaktionsgleichung

5-(4-chlorophenyl)-3,3,6,7-tetramethyl-1H-thieno[2,3-e][1,4]diazepin-2(3H)-one

Lawesson's Reagent

→

5-(4-chlorophenyl)-3,3,6,7-tetramethyl-1H-thieno[2,3-e][1,4]diazepine-2(3H)-thione

Lösungsmittel

Toluene

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux 4 h
2. 2
   EinengenThe solution was concentrated
3. 3
   Sonstigepurified by column chromatography (eluting with hexanes/ethyl acetate)

Vorschrift

A round bottomed flask was charged with 5-(4-chlorophenyl)-3,3,6,7-tetramethyl-1H-thieno[2,3-e][1,4]diazepin-2(3H)-one (324 mg, 0.973 mmol) and a stir bar. Toluene (20 mL, 0.05 M) was added, followed by Lawesson's Reagent (217 mg, 0.535 mmol, 0.55 equiv), and the solution stirred at reflux 4 h. The solution was concentrated and purified by column chromatography (eluting with hexanes/ethyl acetate) to yield 5-(4-chlorophenyl)-3,3,6,7-tetramethyl-1H-thieno[2,3-e][1,4]diazepine-2(3H)-thione as a yellow amorphous solid (m/z=349) that was used in the subsequent reaction.

Quelle