반응 #170174

반응 방정식

1-Chloroethyl chloroformate

1-benzhydryl-3-butoxyazetidine

methanol

→

oil

수율 90.0%

3-Butoxyazetidine hydrochloride

수율 90.0%

용매

1,2-dichloroethane

반응 조건

후처리

1. 1
   온도After cooling down to room temperature
2. 2
   온도The reaction mixture was again heated up to 70° C.
3. 3
   workup.STIRRINGstirred for an additional 1.5 hours
4. 4
   농축After concentration to dryness
5. 5
   기타the crude mixture was triturated in pentane (2×5 mL)

실험 절차

1-Chloroethyl chloroformate (180 μL, 1.6 mmol) was added to a solution of 1-benzhydryl-3-butoxyazetidine (370 mg, 1.2 mmol) in 1,2-dichloroethane (6 mL) at room temperature. The reaction mixture was then heated up to 70° C. and stirred for 1.5 hours. After cooling down to room temperature, methanol (7 mL) was added. The reaction mixture was again heated up to 70° C. and stirred for an additional 1.5 hours. After concentration to dryness, the crude mixture was triturated in pentane (2×5 mL) to give a yellow oil (179 mg, 86%) which was used in the next step without further purification.

출처