Oxygen → 3-Ethyl-2,4-pentanediol
反応式
O=O.[H-].[H-].[H-].[H-].[Li+].[Al+3].[CH2:9]([CH:11]([C:15](=[O:17])[CH3:16])[C:12](=[O:14])[CH3:13])[CH3:10].[OH-].[Na+]>N#N.C1COCC1.O>[CH2:9]([CH:11]([CH:15]([OH:17])[CH3:16])[CH:12]([OH:14])[CH3:13])[CH3:10]参加物
8
実験手順
In N2 atmosphere free of water and oxygen, to a reactor were successively added 0.024 mol LiAlH4 and 100 ml THF, followed by adding dropwise 0.04 mol 3-ethyl-2,4-pentandione while cooling the mixture with ice-bath. The reaction was allowed to continue at room temperature for 48 hours. Aqueous solution of sodium hydroxide was added carefully to stop the reaction. The reaction mixture was filtered and the cake was washed with anhydrous ethyl ether for three times. The organic phase was combined and dried over anhydrous sodium sulfate. Removing the solvent gave 3.4 g product.
後処理
- temperaturewhile cooling the mixture with ice-bath
- customthe reaction
- filtrationThe reaction mixture was filtered
- washthe cake was washed with anhydrous ethyl ether for three times
- dry with materialdried over anhydrous sodium sulfate
- customRemoving the solvent
出典と根拠
- ORDレコード
- ord-10f2cc159f3e4c45981540408442cd7c
- 出典データセット
- uspto-grants-2008_06
- 特許番号
- US07388061B2
反応ノート
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