反应详情

0.72 ml of diisopropylethylamine (4.10 mmol) and 0.16 ml of methoxymethyl chloride (2.05 mmol) were added to a solution of 400 mg of 4-(2-hydroxyphenyl)-2,2-dimethyl-5-oxopiperazine-1-carboxylic acid t-butyl ester obtained in Example (10d) (1.36 mmol) in methylene chloride (14 ml), and the mixture was stirred at room temperature overnight. Water was added to the reaction mixture, followed by extraction with methylene chloride. Then, the organic layer was washed with brine and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:n-hexane/ethyl acetate=1/1) to obtain 497 mg of 2,2-dimethyl-4-(2-methoxymethoxyphenyl)-5-oxopiperazine-1-carboxylic acid t-butyl ester (yield: quant.).

1. extractionfollowed by extraction with methylene chloride
2. washThen, the organic layer was washed with brine
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (elution solvent:n-hexane/ethyl acetate=1/1)