반응식
C(OP([CH:9]1[S:13][CH2:12][CH2:11][S:10]1)(OCC)=O)C.CCCCCC.C([Li])CCC.[CH:25]1[CH:30]=[CH:29][C:28]([C:31]([CH2:33][CH2:34][O:35][C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=O)=[CH:27][CH:26]=1.[Cl-].[Na+]>O1CCCC1>[O:35]([C:34]1[CH:26]=[CH:27][C:28]([C:29](=[C:9]2[S:10][CH2:11][CH2:12][S:13]2)[CH2:30][CH3:25])=[CH:31][CH:33]=1)[C:36]1[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=1참가 물질
실험 절차
2-Diethoxyphosphoryl-1,3-dithiolan, 3.0 g, was dissolved in 30 ml of tetrahydrofuran and 7.75 ml of 1.6 mole hexane solution of n-butyl lithium was dropwise added to the solution in an argon flow at -65° C. The mixture was stirred at the same temperature for an hour. Then, a solution of 2.55 g of 4-phenoxypropiophenone in 9 ml of tetrahydrofuran was dropwise added to the mixture at the same temperature. The reaction mixture was gradually warmed to room temperature overnight. This suspension was poured onto saturated sodium chloride aqueous solution and the mixture was extracted with chloroform. After drying the chloroform phase over magnesium sulfate, the solvent was distilled off under reduced pressure and the residue was purified by silica gel column chromatography (chloroform : hexane =1 : 1) to give 2.60 g of the product.
후처리
- extractionthe mixture was extracted with chloroform
- dry with materialAfter drying the chloroform phase over magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography (chloroform : hexane =1 : 1)
출처 및 근거
- ORD 기록
- ord-40b7a1c835c347f9958e3d3f188c45bc
- 출처 데이터셋
- uspto-grants-1992_03
- 특허 번호
- US05098928
연결된 노트
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