반응 #69553

반응 방정식

N,N-dimethylformamide

3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-6-methoxypyrazolo[5,1-b][1,3]thiazole-7-amine

1-ethyl-3-(3-dimethylaminopropyl)carbodiimide

1-hydroxybenzotriazole

→

title compound

N-{3-[2,6-Dimethoxy-4-(methoxymethyl)phenyl]-6-methoxypyrazolo[5,1-b][1,3]thiazol-7-yl}-1-hydroxycyclopropanecarboxamide

용매

Water

n-heptane ethyl acetate

반응 조건

후처리

1. 1
   추출the reaction mixture was extracted with ethyl acetate
2. 2
   건조dried over anhydrous magnesium sulfate
3. 3
   여과The mixture was filtered
4. 4
   workup.DISTILLATIONthe solvent in the filtrate was distilled off under reduced pressure
5. 5
   기타The residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate

실험 절차

To a N,N-dimethylformamide (6 mL) solution of 3-[2,6-dimethoxy-4-(methoxymethyl)phenyl]-6-methoxypyrazolo[5,1-b][1,3]thiazole-7-amine (400 mg, 1.14 mmol) were added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (0.236 mL, 1.33 mmol) and 1-hydroxybenzotriazole (180 mg, 1.33 mmol), and the mixture was stirred at room temperature over one day and night. Water was added to the reaction mixture, and the reaction mixture was extracted with ethyl acetate and dried over anhydrous magnesium sulfate. The mixture was filtered, and then the solvent in the filtrate was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (a mixed solvent of n-heptane and ethyl acetate: n-heptane/ethyl acetate=1/1 then 1/2) to obtain the title compound (404 mg, 0.93 mmol).

출처