반응 #42081

반응 방정식

HCl

product

N-[3-Acetyl-6-(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-2-oxo-1,2-dihydro-1,8-naphthyridin-4-yl]acetamide

HCl

→

3-Acetyl-4-amino-6-(4-chlorophenyl)-7-(2,4-dichlorophenyl)-1-methyl-1,8-naphthyridin-2(1H)-one

용매

EtOAc

1,4-dioxane

반응 조건

후처리

1. 1
   기타forming
2. 2
   온도The temperature was increased to 90° C. for 4.5 hours at which
3. 3
   온도was cooled to room temperature
4. 4
   세척The solution was washed with saturated aqueous NaHCO3 solution
5. 5
   건조before drying with Na2SO4
6. 6
   농축concentrating
7. 7
   기타The residue was purified by preparative TLC (silica gel)
8. 8
   세척eluted with 20% EtOAc in CH2Cl2 affording the title compound

실험 절차

To 16 mg of the product of Example 1 in 1,4-dioxane (1 mL) was added 0.5 mL of 1 M aqueous HCl solution. The reaction stirred at 50° C. for 5 hours. LC/MS indicated little product forming and an additional 0.2 mL of concentrated HCl solution was added. The temperature was increased to 90° C. for 4.5 hours at which point the reaction was cooled to room temperature and diluted with EtOAc. The solution was washed with saturated aqueous NaHCO3 solution before drying with Na2SO4 and concentrating. The residue was purified by preparative TLC (silica gel) eluted with 20% EtOAc in CH2Cl2 affording the title compound. HPLC/MS: 471.9 (M+1), 473.9 (M+3); Rt=4.32 min.

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