Reaktion #40668

Reaktionsgleichung

2e

2-(3,3-dimethylindolin-1-yl)benzenamine

benzoyl isothiocyanate

→

2f

Ausbeute 112.7%

1-benzoyl-3-(2-(3,3-dimethylindolin-1-yl)phenyl)thiourea

Ausbeute 112.7%

Lösungsmittel

CH2Cl2

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux for 2.5 h
2. 2
   FiltrationThe reaction mixture was filtered through a cake of Celite®
3. 3
   Waschenwashed the cake with CH2Cl2
4. 4
   SonstigeThe solvent was evaporated under reduced pressure
5. 5
   SonstigeThe desired product was purified by column chromatography
6. 6
   Sonstigeover 60 min
7. 7
   Waschenas eluting gradient

Vorschrift

To a solution of 2e (40 mg, 0.168 mmol) in CH2Cl2 was added benzoyl isothiocyanate (30 mg, 0.189 mmol). The reaction mixture was kept at reflux for 2.5 h. The reaction mixture was filtered through a cake of Celite® and washed the cake with CH2Cl2. The solvent was evaporated under reduced pressure. The desired product was purified by column chromatography using 0 to 80% EtOAc in hexane over 60 min as eluting gradient to afford 2f (76 mg, 99%) as a powder. MS (ES) m/z 402 [M+H]+.

Quelle