반응 #2259168

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

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

1,2-dichloroethane

1-Chloroethyl chloroformate

→

3-(2-Thienylmethoxy)azetidine hydrochloride

용매

methanol

반응 조건

후처리

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

실험 절차

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.

출처