반응 #54955
ord-040e02245ccf4febaf7f5fc948a20887
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용매
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후처리
- 1추출the mixture was extracted with chloroform (4×70 ml)
- 2추출The combined chloroform phases were extracted with saturated sodium bicarbonate solution (4×30 ml)
- 3세척washed with chloroform (100 ml)
- 4추출The precipitated product was extracted with chloroform (3×100 ml)
- 5건조the combined extracts dried over magnesium sulphate
- 6기타After removing solvent
- 7기타the product was recrystallised from benzene/hexane (1;1)
실험 절차
2-(2-Ethyl-4-oxo-4H-1-benzopyran-6-yl)propan-1-ol (3.0 g; 0.0129 mol) was dissolved in acetone (20 ml) and Jones Reagent (Example 2) was slowly added until the solution attained a permanent brown colour. Water (100 ml) was added and the mixture was extracted with chloroform (4×70 ml). The combined chloroform phases were extracted with saturated sodium bicarbonate solution (4×30 ml). The aqueous phases were combined, washed with chloroform (100 ml) and then acidified with concentrated hydrochloric acid. The precipitated product was extracted with chloroform (3×100 ml) and the combined extracts dried over magnesium sulphate. After removing solvent, the product was recrystallised from benzene/hexane (1;1) to yield a pale yellow amorphous solid (1.4 g) mp 128°-128.5°.