Triethylsilane → HCID 24864236、化合物
反応式
[CH3:1][C:2]1([CH3:14])[O:6][C@H:5]([CH2:7][C:8](=[O:12])SCC)[C:4](=[O:13])[O:3]1.C([SiH](CC)CC)C>C(Cl)Cl.[Pd]>[CH3:1][C:2]1([CH3:14])[O:6][C@H:5]([CH2:7][CH:8]=[O:12])[C:4](=[O:13])[O:3]1参加物
5
実験手順
(R)—S-Ethyl 2-(2,2-dimethyl-5-oxo-1,3-dioxolan-4-yl)ethanethioate (22.5 g, 103 mmol) was dissolved in CH2Cl2 (500 mL), purged with nitrogen and 10% palladium on carbon (2.19 g, 2.06 mmol) was added and triethylsilane (24.7 mL, 155 mmol) was dissolved in CH2Cl2 (20 mL) and added dropwise through an addition funnel over 30 minutes and stirred at ambient temperature overnight under nitrogen. The reaction was filtered through celite, concentrated and purified over silica gel (10 to 40% EtOAc in hexanes) to afford (R)-2-(2,2-dimethyl-5-oxo-1,3-dioxolan-4-yl)acetaldehyde (16 g, 101 mmol, 98.1% yield) as a clear colorless oil.
後処理
- additionwas added
- additionadded dropwise through an addition funnel over 30 minutes
- filtrationThe reaction was filtered through celite,
- concentrationconcentrated
- custompurified over silica gel (10 to 40% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-5579effdb07540a5849ba76d8695aa48
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754226B2
反応ノート
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