Reaktion #170217

Reaktionsgleichung

1-Chloroethyl chloroformate

1-benzhydryl-3-(3,3,3-trifluoropropoxy)-azetidine

Ethanol

→

3-(3,3,3-Trifluoropropoxy)azetidine hydrochloride

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe reaction mixture was stirred for 1 hour at room temperature and for 2 hours at 45° C
2. 2
   EinengenAfter concentration to dryness
3. 3
   Sonstigethe crude mixture was triturated in petroleum ether (2×20 mL)
4. 4
   Sonstigeto give a yellow oil (245 mg, quantitative) which
5. 5
   Sonstigewas used in the next step without further purification

Vorschrift

1-Chloroethyl chloroformate (136 μL, 1.25 mmol) was added to a solution of 1-benzhydryl-3-(3,3,3-trifluoropropoxy)-azetidine (400 mg, 1.19 mmol) in dichloromethane (10 mL) at 0° C. The reaction mixture was stirred for 1 hour. Ethanol (10 mL) was added and the reaction mixture was stirred for 1 hour at room temperature and for 2 hours at 45° C. After concentration to dryness, the crude mixture was triturated in petroleum ether (2×20 mL) to give a yellow oil (245 mg, quantitative) which was used in the next step without further purification.

Quelle