1-(氯甲基)-3-碘苯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-iodobenzyl chloride (100 mg, 0.396 mmol) in 1,4-dioxane (3 ml) was treated with pyrrolidine (0.5 ml, 6.02 mmol) and heated to reflux for 5 h. The cooled mixture was evaporated to dryness and treated with EtOAc and water. The organics were separated, dried over MgSO4, filtered and evaporated to afford 1-(3-iodo-benzyl)-pyrrolidine as a clear syrup (110 mg, 97%). heated to reflux for 5 h The cooled mixture was evaporated to dryness treated with EtOAc and water The organics were separated dried over MgSO4 filtered evaporated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 3-iodobenzyl alcohol (600 mg, 2.56 mmol) in DCM (3 ml) was treated with thionyl chloride (3 ml, 41.3 mmol) and stirred at ambient temperature for 18 h, before addition of further thionyl chloride (1 ml, 13.7 mmol) and heating to reflux for 12 h. The cooled solution was basified with 50% NaOH, diluted with water and extracted with DCM. The combined organics were dried over MgSO4, filtered and evaporated to afford a clear syrup which crystallises on standing to give 3-iodobenzyl chloride as a white solid (650 mg, quant.). heating to reflux for 12 h extracted with DCM The combined organics were dried over MgSO4 filtered evaporated to afford a clear syrup which crystallises