반응 #476247

반응 방정식

Triethylamine

7-bromo-4-hydroxyquinolin-3-aminium chloride

Acetoxyacetyl chloride

→

2-[(7-bromo-4-hydroxyquinolin-3-yl)amino]-2-oxoethyl acetate

수율 80.7%

용매

dichloromethane

반응 조건

후처리

1. 1
   workup.WAITto stand for three days
2. 2
   기타was isolated by filtration
3. 3
   기타pressed dry
4. 4
   workup.STIRRINGThe solid was stirred in deionized water (2 L) for two hours
5. 5
   기타isolated by filtration
6. 6
   기타dried overnight on the filter funnel
7. 7
   기타further dried in a vacuum oven at 60 to 70° C.

실험 절차

Triethylamine (161 g, 1.59 mol) was added to a suspension of 7-bromo-4-hydroxyquinolin-3-aminium chloride (224 g, 0.815 mol) in dichloromethane (2.25 L), and the mixture was cooled to approximately 0° C. Acetoxyacetyl chloride (112 g, 0.820 mol) was added over a period of one hour. The reaction was stirred at room temperature for one hour and then allowed to stand for three days. A solid was present and was isolated by filtration and pressed dry. The solid was stirred in deionized water (2 L) for two hours, isolated by filtration, dried overnight on the filter funnel, and further dried in a vacuum oven at 60 to 70° C. to provide 223 g of 2-[(7-bromo-4-hydroxyquinolin-3-yl)amino]-2-oxoethyl acetate as a reddish brown solid.

출처