반응식
ClC1C=CC=C(C(OO)=O)C=1.S([O-])([O-])(=O)=O.[Mg+2].B(F)(F)F.CCOCC.[CH2:27]([O:29][C:30](=[O:44])[C:31]1[CH:36]=[CH:35][C:34]([CH:37]2[CH2:41][CH:40]([O:42]C)[O:39][CH2:38]2)=[CH:33][CH:32]=1)[CH3:28]>ClCCl.CCOCC>[CH2:27]([O:29][C:30](=[O:44])[C:31]1[CH:32]=[CH:33][C:34]([CH:37]2[CH2:41][C:40](=[O:42])[O:39][CH2:38]2)=[CH:35][CH:36]=1)[CH3:28]참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
To a solution of 75% 3-chloroperbenzoic acid (2.7 g, 11.76 mmol) in dichloromethane (35 mL) is added magnesium sulfate (2.0 g, 16.6 mmol) and the mixture stirred for 30 min. Solids are removed by filtration and the filtrate treated with borontrifluoride etherate (0.5 mL, 3.92 mmol) and 4-(5-methoxy-tetrahydro-furan-3-yl)-benzoic acid ethyl ester (2.45 g, 9.8 mmol) in dichloromethane (5 mL). The mixture is stirred at room temperature 18 h, diluted with ether (200 mL) and washed with a 10% solution of sodium thiosulfite (150 mL), a saturated solution of sodium bicarbonate (150 mL) and brine. The mixture is dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is chromatographed on SiO2 (elute with 20% ethyl acetate/hexanes) to yield the title compound, 2.2 g (96%), as an off-white solid.
후처리
- customSolids are removed by filtration
- stirringThe mixture is stirred at room temperature 18 h
- washwashed with a 10% solution of sodium thiosulfite (150 mL)
- dry with materialThe mixture is dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue is chromatographed on SiO2 (elute with 20% ethyl acetate/hexanes)
출처 및 근거
- ORD 기록
- ord-533050e5611d4df3b3683b95512ad06a
- 출처 데이터셋
- uspto-grants-2006_08
- 특허 번호
- US07087626B2
연결된 노트
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