Reaktion #535944

Reaktionsgleichung

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride

1-[(2-benzothienylcarbonyl)amino]cyclohexanecarboxylic acid

→

title compound

Ausbeute 76.7%

2-(2-Benzothienyl)-3-oxa-1-azaspiro[4.5]dec-1-en-4-one

Ausbeute 76.7%

Lösungsmittel

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenthe reaction solution was concentrated under reduced pressure, ethyl acetate
2. 2
   workup.ADDITIONwas added
3. 3
   Waschenthe mixture was successively washed with water
4. 4
   TrocknenThe organic layer was dried with anhydrous sodium sulfate
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure

Vorschrift

4.1 g (21 mmol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride was added to a solution of 5 g (16 mmol) of 1-[(2-benzothienylcarbonyl)amino]cyclohexanecarboxylic acid in 50 ml of methylene chloride. After the mixture was stirred at room temperature for 4 hours, the reaction solution was concentrated under reduced pressure, ethyl acetate was added thereto, and the mixture was successively washed with water, a 10% aqueous potassium hydrogensulfate solution, a saturated aqueous sodium hydrogencarbonate solution and saturated brine. The organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off under reduced pressure to obtain 3.5 g (75%) of the title compound.

Quelle