Reaktion #170112

Reaktionsgleichung

1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine

1-(Diphenylmethyl)-3-(2-thienylmethoxy)azetidine

1,2-dichloroethane

1-Chloroethyl chloroformate

→

3-(2-Thienylmethoxy)azetidine hydrochloride

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturAfter cooling to room temperature
2. 2
   workup.STIRRINGthe reaction mixture was stirred at 70° C. for 1.5 h
3. 3
   EinengenThe reaction mixture was concentrated to dryness
4. 4
   SonstigeThe crude mixture was triturated in pentane
5. 5
   Sonstigeto give a dark wax (140 mg, quantitative) which
6. 6
   Sonstigewas used without further purification

Vorschrift

A 50 mL flask was charged with 1-(diphenylmethyl)-3-(2-thienylmethoxy)azetidine (204 mg, 0.61 mmol; which may be prepared as described in Step 2) and 1,2-dichloroethane (2.7 mL). 1-Chloroethyl chloroformate (86 μL, 0.79 mmol) was added and the reaction mixture was stirred at 70° C. for 1.5 h. After cooling to room temperature, methanol (2.7 mL) was added and the reaction mixture was stirred at 70° C. for 1.5 h. The reaction mixture was concentrated to dryness. The crude mixture was triturated in pentane to give a dark wax (140 mg, quantitative) which was used without further purification.

Quelle