反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([Mg]Br)=[CH:5][CH:4]=1.[CH2:11]([O:18][C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]=[O:22])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-].[NH4+]>C1COCC1>[CH2:11]([O:18][C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[CH:21]([C:6]1[CH:7]=[CH:8][C:3]([S:2][CH3:1])=[CH:4][CH:5]=1)[OH:22])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1参加物
実験手順
In a nitrogen stream, a solution of 4-methylsulfanyl-phenylmagnesium bromide in THF (0.5 M, 35 mL) was added dropwise to a solution of 2-benzyloxybenzaldehyde (2.60 g, 12.2 mmol) in THF (24 mL) at 0° C. and the mixture was stirred at room temperature for two hours, and then a saturated ammonium chloride aqueous solution was added thereto under cooling with ice and the mixture was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride aqueous solution and dried (anhydrous magnesium sulfate), and then the solvent was distilled under reduced pressure. The obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate:n-hexane (1:4)] to obtain the title compound (3.91 g, 95%).
後処理
- temperatureunder cooling with ice
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with a saturated sodium chloride aqueous solution
- dry with materialdried (anhydrous magnesium sulfate)
- distillationthe solvent was distilled under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography [developing solution=ethyl acetate:n-hexane (1:4)]
出典と根拠
- ORDレコード
- ord-e56e184b5ef54d4f90254602f3a895b4
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08048897B2
関連ノート
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