Реакция #66504

Уравнение реакции

3-iodo-4-methylbenzoyl chloride

methylamine

THF

→

3-iodo-N,4-dimethylbenzamide

Выход 95.0%

Растворители

DCM

Условия реакции

Обработка

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

Методика

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.

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