Reaktion #721124

Reaktionsgleichung

1-Chloroethyl chloroformate

1-benzhydryl-3-((3-methylthiophen-2-yl)methoxy)azetidine

Ethanol

→

3-((3-Methylthiophen-2-yl)methoxy)azetidine hydrochloride

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstige30 minutes
2. 2
   Sonstigeat room temperature
3. 3
   workup.STIRRINGthe reaction mixture was stirred at 35° C. for an additional 3 hours
4. 4
   EinengenAfter concentration to dryness
5. 5
   Sonstigethe crude was triturated in pentane
6. 6
   Sonstigeto give a yellow solid (200 mg, quantitative) which
7. 7
   Sonstigewas used in the next step without further purification

Vorschrift

1-Chloroethyl chloroformate (90 μL, 0.84 mmol) was added to a solution of 1-benzhydryl-3-((3-methylthiophen-2-yl)methoxy)azetidine (290 mg, 0.83 mmol) in dichloromethane (9 mL) at 0° C. The reaction mixture was stirred 3 hours, then 30 minutes at room temperature. Ethanol (9 mL) was added and the reaction mixture was stirred at 35° C. for an additional 3 hours. After concentration to dryness, the crude was triturated in pentane to give a yellow solid (200 mg, quantitative) which was used in the next step without further purification.

Quelle