反应 #3103391
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09321769B2
反应条件: temp:70.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 1-Chloroethyl chloroformate (210 μL, 1.9 mmol) was added to a solution of 1-benzhydryl-3-(3-methoxypropoxy)-azetidine (460 mg, 1.5 mmol) in 1,2-dichloroethane (7 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 and the mixture was again warmed up to 70° C. and stirred for an additional 2 hours. After concentration to dryness, the crude was triturated in pentane (2×10 mL) to afford a yellow oil (247 mg, 92%) which was used in the next step without further purification. After cooling down to room temperature the mixture was again warmed up to 70° C. stirred for an additional 2 hours After concentration to dryness the crude was triturated in pentane (2×10 mL)
来源 ID: ord-69b68423ecc94abcabd66c976af0d403