반응 #1563875
ord-fac823e27f7d4f01835b164bc872d328
반응 방정식
반응 조건
후처리
- 1건조dried over KOH
- 2온도the resulting ethereal solution was cooled in an ice-salt bath
- 3기타The solvent was evaporated to dryness (under an argon atmosphere
- 4기타the water bath temperature below 25° C.
- 5기타was purified by column chromatography
- 6기타Evaporation of solvent
실험 절차
N-Nitroso-N-methylurea (16.14 g, 61.53 mmol) was treated with a concentrated NaOH aqueous solution to produce diazomethane. The diazomethane was combined with dry ether (100 ml), dried over KOH, and the resulting ethereal solution was cooled in an ice-salt bath. A solution of furan-2-carbonyl chloride (1.6 g, 12.3 mmol) in dry ether (25 ml) was then added very slowly to the diazomethane solution. The reaction mixture was stirred overnight at room temperature. The solvent was evaporated to dryness (under an argon atmosphere, and keeping the water bath temperature below 25° C.), and the resulting crude material was purified by column chromatography using 230-400 mesh silica gel and 1% triethylamine in DCM solvent system. Evaporation of solvent yielded 2-diazo-1-(furan-2-yl)ethanone as a yellow oil (900 mg, 49%).