HRID735022

反应详情

EQUATION

反应方程式

HRID 735022 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

3 mL (38.76 mmol) of trifluoroacetic acid are added to a solution of 1 g (2.78 mmol) of tert-butyl [1-(4-iodophenyl)cyclopropyl]carbamate in 40 mL dichloromethane and stirred for 24 h. Then the solvent is eliminated by rotary evaporation and the residue is combined with toluene and then again eliminated by rotary evaporation. This residue is then added to a solution of 0.39 g (2.8 mmol) of potassium carbonate in 20 mL of water and stirred for 30 minutes at RT. The aqueous phase is extracted with dichloromethane, the organic phase is dried with sodium sulfate and the solvent is eliminated by rotary evaporation. Yield: 0.7 g (97% of theory); C9H10IN (M=259.09); calc.: molecular ion peak (M+H)+: 260; found: molecular ion peak (M+H)+: 260.

WORKUP

后处理

  1. customThen the solvent is eliminated by rotary evaporation
  2. customagain eliminated by rotary evaporation
  3. stirringstirred for 30 minutes at RT
  4. extractionThe aqueous phase is extracted with dichloromethane
  5. dry with materialthe organic phase is dried with sodium sulfate
  6. customthe solvent is eliminated by rotary evaporation