Reaktion #472199

Reaktionsgleichung

2,3-dihydro-1,3-benzothiazole

2-aminobenzenethiol

formalin

3-cyano-4-methoxy-5-trifluoromethylbenzoylchloride

→

3-(3-cyano-4-methoxy-5-trifluoromethylbenzoyl)-2,3-dihydro-1,3-benzothiazole

Lösungsmittel

chloroform

triethylamine

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure and water
2. 2
   workup.ADDITIONwas added
3. 3
   Extraktionthe mixture was extracted with ethyl acetate
4. 4
   WaschenThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
5. 5
   Trocknendried over anhydrous sodium sulfate
6. 6
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
7. 7
   Sonstigethe obtained residue was used for the synthesis of (j)

Vorschrift

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (5.00 g) and 37% formalin (3.0 mL) in the same manner as in the synthesis of Example 1 was dissolved in chloroform (50 mL), and triethylamine (11.1 mL) and 3-cyano-4-methoxy-5-trifluoromethylbenzoylchloride were added to the solution, and then the mixture was stirred at room temperature for 1 hour. The solvent was distilled off under reduced pressure and water was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (j).

Quelle