反应详情

In 2 ml of ethanol was dissolved 50 g (0.17 mmol)of 5-(3,5-dimethylphenylthio)-4-isopropyl-1-methyl-1H-imidazole-2-carbaldehyde (Compound I-6), followed by addition of 36 mg (0.5 mmol)of hydroxylamine hydrochloride and 43 mg (0.5 mmol) of sodium acetate, and the mixture was stirred for 30 minutes at room temperature. To this reaction mixture, water was added, and the mixture was extracted with methylene chloride. The organic layer was washed with water, dried over sodium sulfate, and the solvent was concentrated under reduced pressure. The residue was washed with ethyl acetate to precipitate the product, and 32 mg (yield 60%)of Compound I-10 was obtained by the filtration. mp 240-241° C.

1. extractionthe mixture was extracted with methylene chloride
2. washThe organic layer was washed with water
3. dry with materialdried over sodium sulfate
4. concentrationthe solvent was concentrated under reduced pressure
5. washThe residue was washed with ethyl acetate
6. customto precipitate the product