반응 #76519

반응 방정식

product

[(1,2,3,4-Tetrahydro-6-nitro-5-quinolinyl)amino]oxo-acetic acid ethyl ester

N-bromosuccinimide

→

title compound

수율 81.0%

[(8-Bromo-1,2,3,4-tetrahydro-6-nitro-5-quinolinyl)-amino]oxo-acetic acid ethyl ester

수율 81.0%

용매

dimethylformamide

반응 조건

후처리

1. 1
   workup.ADDITIONThe solution was poured onto methylene chloride/water
2. 2
   기타separated
3. 3
   추출the water layer back extracted with methylene chloride
4. 4
   세척The combined organic layers were washed with water
5. 5
   건조dried over sodium sulfate
6. 6
   여과filtered
7. 7
   기타evaporated
8. 8
   기타The residue was purified by silica gel chromatography (4:1 to 1:1 heptane:ethyl acetate as eluant)

실험 절차

A mixture of the product from Example 87 (0.15 g, 0.5 mmol) and N-bromosuccinimide (0.23 g, 1 mmol) in 2 mL dimethylformamide was stirred at room temperature for 18 hours. The solution was poured onto methylene chloride/water and separated and the water layer back extracted with methylene chloride. The combined organic layers were washed with water, dried over sodium sulfate, filtered and evaporated. The residue was purified by silica gel chromatography (4:1 to 1:1 heptane:ethyl acetate as eluant) to give the title compound (0.15 g, 81% yield).

출처