Water → 2-(2,2-Diethoxyethyl)-1,3-propanediol

HRID 1111375ノート

反応式

HRID 1111375 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([O:9][CH:10]([O:23][CH2:24][CH3:25])[CH2:11][CH:12]([C:18](OCC)=[O:19])[C:13](OCC)=[O:14])[CH3:8].O.[OH-].[Na+]>O1CCCC1>[CH2:24]([O:23][CH:10]([O:9][CH2:7][CH3:8])[CH2:11][CH:12]([CH2:13][OH:14])[CH2:18][OH:19])[CH3:25]

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 298328Diethyl 3,3-Diethoxypropane-1,1-dicarboxylateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 122006482-(2,2-Diethoxyethyl)-1,3-propanediol収率 71.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a cooled suspension (0° C.) of lithium aluminum hydride (4.9 g, 0.129 mol) in anhydrous tetrahydrofuran (80 mL), was added a solution of diethyl 2,2-diethoxyethylmalonate (17.6 g, 63.7 mmol) in anhydrous tetrahydrofuran (60 mL), and the mixture was stirred 3 h at room temperature. Then, the reaction mixture was immersed in an ice bath and a mixture of water (4.6 mL) and tetrahydrofuran (9.2 mL) was added dropwise followed by a solution of 15% sodium hydroxide (4.6 mL) and water (12.5 mL). After stirring for 20 minutes, the suspension was filtered off, the solvent was removed at reduced pressure, and 300 mL of chloroform was added. The solution was dried over sodium sulfate and after removal of the solvent, 8.8 g of a white solid was obtained and used in the next step without further purification.

後処理

  1. customThen, the reaction mixture was immersed in an ice bath
  2. additionwas added dropwise
  3. stirringAfter stirring for 20 minutes
  4. filtrationthe suspension was filtered off
  5. customthe solvent was removed at reduced pressure, and 300 mL of chloroform
  6. additionwas added
  7. dry with materialThe solution was dried over sodium sulfate
  8. customafter removal of the solvent

出典と根拠

ORDレコード
ord-675c20109fc94598b420f3514411c556
出典データセット
uspto-grants-1990_12
特許番号
US04980362

反応ノート

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