Diethyl Ether → HCID 21866824、化合物
反応式
CCOCC.[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:12][CH2:13][CH2:14][CH2:15][CH2:16][CH:17]([C:23](OCC)=[O:24])[C:18](OCC)=[O:19].[OH-].[Na+]>O.O1CCCC1>[Cl:12][CH2:13][CH2:14][CH2:15][CH2:16][CH:17]([CH2:23][OH:24])[CH2:18][OH:19]参加物
7
実験手順
To 214 ml of dry ether was added 8 g of lithium aluminium hydride, and a solution of 26.7 g of diethyl (4-chlorobutyl)malonate/53 ml of dry ether was added dropwise with stirring under ice-cooling. After 1-hour-stirring at room temperature, the mixture was cooled with ice-cold water, and 173 ml of tetrahydrofuran/14.7 ml of water was added gradually. Then, 14.7 ml of 1N sodium hydroxide solution and 35 ml of water were added, stirred for 15 minutes, filtrated to remove insolubles. The filtrate was concentrated to provide 18.2 g of the objective compound as colorless oil.
後処理
- temperaturecooling
- stirringAfter 1-hour-stirring at room temperature
- additionwas added gradually
- stirringstirred for 15 minutes
- filtrationfiltrated
- customto remove insolubles
- concentrationThe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-fb14c63a73bf4a30964e53f49506e515
- 出典データセット
- uspto-grants-2006_04
- 特許番号
- US07022723B2
反応ノート
読み込み中…
