반응식
[CH3:1][Li].[C:3]([C:6]1[CH:14]=[CH:13][C:9]2[O:10][CH2:11][O:12][C:8]=2[CH:7]=1)(=[O:5])[CH3:4].O>O1CCCC1>[O:10]1[C:9]2[CH:13]=[CH:14][C:6]([C:3]([OH:5])([CH3:1])[CH3:4])=[CH:7][C:8]=2[O:12][CH2:11]1참가 물질
5
반응 조건
- 온도
- -20 °C
실험 절차
About 600 ml of 1.5M methyllithium (solution in ether) was added to 500 ml of tetrahydrofuran. A suspension of 93.45 g of 5-acetyl-1,3-benzodioxole in 900 ml of tetrahydrofuran was added thereto under cooling at -20° C. The mixture was stirred under these conditions for 1 h. Water was added to the reaction mixture. The product was extracted with ethyl acetate, washed with a saturated aqueous common salt solution and dried over anhydrous magnesium sulfate. After filtration, the filtrate was concentrated to obtain 97 g of the intended compound in the form of an oil.
후처리
- additionwas added
- extractionThe product was extracted with ethyl acetate
- washwashed with a saturated aqueous common salt solution
- dry with materialdried over anhydrous magnesium sulfate
- filtrationAfter filtration
- concentrationthe filtrate was concentrated
출처 및 근거
- ORD 기록
- ord-d359b559f57a4cdc9504feb94d8a3821
- 출처 데이터셋
- uspto-grants-1994_03
- 특허 번호
- US05292901
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