반응 #45815

반응 방정식

N-Bromosuccinimide

N,N-dimethylformamide

methyl 4-acetylaminosalicylate

→

compound

수율 45.0%

Methyl 4-acetylamino-5-bromosalicylate

수율 45.0%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도with heating
2. 2
   온도After cooling to room temperature
3. 3
   세척by washing twice with saturated brine
4. 4
   건조drying over anhydrous magnesium sulfate
5. 5
   여과After filtration and concentration under reduced pressure

실험 절차

N-Bromosuccinimide (0.94 g, 5.3 mmol) was added to an N,N-dimethylformamide (8 ml) solution of methyl 4-acetylaminosalicylate (I-248) (1.1 g, 5.0 mmol), followed by stirring with heating under reflux at 70 to 75° C. for 2 hours and a half. After cooling to room temperature, ethyl acetate was added, followed by washing twice with saturated brine and drying over anhydrous magnesium sulfate. After filtration and concentration under reduced pressure, the resulting residue was subjected to column chromatography, and the eluate with chloroform/methanol (100:1) gave the entitled compound (0.64 g, 45%) as a pale red solid.

출처