Reaktion #2251388

Reaktionsgleichung

2,2-dimethyl-1,3-benzodithiole-4-sulfonamide

2,2-Dimethyl-1,3-Benzodithiole-4-Sulfonamide

trimethylaluminum

acetic acid

methyl [4-methoxy-6-methyl-1,3,5-triazin-2-yl]carbamate

→

N-[(4-Methoxy-6-methyl-1,3,5-triazin-2-yl)aminocarbonyl]-2,2-dimethyl-1,3-benzodithiole-4-sulfonamide

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added
2. 2
   Temperaturthe reaction mixture was heated
3. 3
   Temperaturat reflux for 72 hours
4. 4
   TemperaturThe reaction mixture was cooled to room temperature
5. 5
   SonstigeThe organic phase was separated
6. 6
   Sonstigedried
7. 7
   Sonstigethe solvent removed under reduced pressure
8. 8
   Sonstigeto give an oil
9. 9
   SonstigeCrystallization of the oil from an appropriate solvent
10. 10
    Sonstigegave a solid

Vorschrift

To a solution of 2.6 g 2,2-dimethyl-1,3-benzodithiole-4-sulfonamide prepared in Example 7, in 60 ml methylene chloride at room temperature under nitrogen is added 5.5 ml trimethylaluminum (2M in toluene). After stirring 15 minutes at room temperature, 2.0 g of methyl [4-methoxy-6-methyl-1,3,5-triazin-2-yl]carbamate, prepared according to the procedure of Example 5, was added and the reaction mixture was heated at reflux for 72 hours. The reaction mixture was cooled to room temperature and 75 ml ice, 3 ml glacial acetic acid, and 10 drops of hydrochloric acid were sequentially added. The organic phase was separated, dried and the solvent removed under reduced pressure to give an oil. Crystallization of the oil from an appropriate solvent gave a solid.

Quelle