반응 #66504

반응 방정식

3-iodo-4-methylbenzoyl chloride

methylamine

THF

→

3-iodo-N,4-dimethylbenzamide

수율 95.0%

용매

DCM

반응 조건

후처리

1. 1
   workup.ADDITIONUpon completion of the addition
2. 2
   기타the ice bath was removed
3. 3
   기타All volatiles were removed in vacuo
4. 4
   workup.ADDITIONthe residue was treated with aq. NaHCO3 (25 mL)
5. 5
   추출subsequently extracted with ethyl acetate (3×15 mL)
6. 6
   건조The combined organic layers were dried over MgSO4
7. 7
   기타evaporated

실험 절차

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.

출처