反応式
[CH3:1][C:2]1[CH2:7][CH2:6][CH2:5][C:4]([CH3:9])([CH3:8])[C:3]=1/[CH:10]=[CH:11]/[C:12]([CH3:14])=[O:13].[SH:15][CH2:16][CH2:17][CH2:18][Si:19]([O:24][CH3:25])([O:22][CH3:23])[O:20][CH3:21].Cl>C1CCN2C(=NCCC2)CC1>[CH3:21][O:20][Si:19]([O:22][CH3:23])([O:24][CH3:25])[CH2:18][CH2:17][CH2:16][S:15][CH:10]([C:3]1[C:4]([CH3:8])([CH3:9])[CH2:5][CH2:6][CH2:7][C:2]=1[CH3:1])[CH2:11][C:12](=[O:13])[CH3:14]参加物
5
実験手順
To a well-stirred mixture of β-ionone (10.00 g, 52.1 mmol) and DBU (79 mg, 0.52 mmol (1 mol-%)) was rapidly added 3-mercaptopropyltrimethoxysilane (10.21 g, 52.1 mmol) at 25-30° C. After 72 hours, the reaction mixture was poured onto a cold stirred 5% aqueous HCl solution and extracted twice with Et2O. The organic phases were washed (H2O, saturated aqueous NaHCO3 and brine), dried (Na2SO4), filtered and concentrated. The crude extract was dried for 1 hour at 65-70° C./0.01 Torr to give 18.00 g of the title thioether containing approximativaly 10% of β-ionone. Yield: 80%.
後処理
- customat 25-30° C
- additionthe reaction mixture was poured onto
- extractionextracted twice with Et2O
- washThe organic phases were washed (H2O, saturated aqueous NaHCO3 and brine)
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated
- extractionThe crude extract
- customwas dried for 1 hour at 65-70° C./0.01 Torr
出典と根拠
- ORDレコード
- ord-f419cbac44c6454b93d26078fa5db95a
- 出典データセット
- uspto-grants-2009_09
- 特許番号
- US07589055B2
関連ノート
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