反応 #66504

反応方程式

3-iodo-4-methylbenzoyl chloride

methylamine

THF

→

3-iodo-N,4-dimethylbenzamide

収率 95.0%

溶媒

DCM

反応条件

後処理

1. 1
   workup.ADDITIONUpon completion of the addition
2. 2
   その他the ice bath was removed
3. 3
   その他All volatiles were removed in vacuo
4. 4
   workup.ADDITIONthe residue was treated with aq. NaHCO3 (25 mL)
5. 5
   抽出subsequently extracted with ethyl acetate (3×15 mL)
6. 6
   乾燥The combined organic layers were dried over MgSO4
7. 7
   その他evaporated

実験手順

To a cooled (0° C.) solution of 3-iodo-4-methylbenzoyl chloride (2.80 g; 10.0 mmol) in DCM (10 mL) was slowly added a 2 M solution of methylamine in THF (11 mL, 2.2 eq.). Upon completion of the addition, the ice bath was removed and the mixture was stirred overnight. All volatiles were removed in vacuo and the residue was treated with aq. NaHCO3 (25 mL) and subsequently extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over MgSO4 and evaporated. The target compound 3-iodo-N,4-dimethylbenzamide (2.62 g, 95% yield) was used without further purification.

出典