反应 #554642

反应方程式

N-(1-(4-bromophenyl)propan-2-yl)acetamide

NaI

→

N-(1-(4-iodophenyl)propan-2-yl)acetamide

溶剂

dioxan

反应条件

后处理

1. 1
   温度to cool to r.t.
2. 2
   其他half of the solvent is removed in vacuo
3. 3
   workup.ADDITIONEtOAc and diluted aq. ammonia solution are added
4. 4
   其他the layers are separated
5. 5
   萃取The aq. layer is once more extracted with EtOAc
6. 6
   干燥dried with Na2SO4
7. 7
   过滤filtered
8. 8
   其他the solvent is removed in vacuo
9. 9
   其他The crude product is triturated with diethylether
10. 10
    其他dried at 50° C. in vacuo

实验过程

To 6.00 g (23.4 mmol) N-(1-(4-bromophenyl)propan-2-yl)acetamide (II.1) in 65 mL dioxan are added 0.45 g (2.34 mmol) CuI, 0.50 mL (4.70 mmol) N,N″-dimethyl-ethylendiamine and 7.02 g (46.9 mmol) NaI. The reaction mixture is stirred at 120° C. for 70 h. The mixture is allowed to cool to r.t. and half of the solvent is removed in vacuo. EtOAc and diluted aq. ammonia solution are added and the layers are separated. The aq. layer is once more extracted with EtOAc. The organic layers are combined, dried with Na2SO4, filtered and the solvent is removed in vacuo. The crude product is triturated with diethylether and dried at 50° C. in vacuo.

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