反応 #69553

反応方程式

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

溶媒

Water

n-heptane ethyl acetate

反応条件

後処理

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

実験手順

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).

出典