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Water → 1,3-Propanediol, 2-(2,2-dimethoxyethyl)-

HRID 2291844
ノート
印刷プレビュー

反応式

HRID 2291844 の反応式
[CH3:1][O:2][CH:3]([O:16][CH3:17])[CH2:4][CH:5]([C:11](OCC)=[O:12])[C:6](OCC)=[O:7].[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>CCOCC>[CH3:17][O:16][CH:3]([O:2][CH3:1])[CH2:4][CH:5]([CH2:11][OH:12])[CH2:6][OH:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962Water2 回HCID 14798Sodium HydroxideHCID 14215238Diethyl (2,2-dimethoxyethyl)malonateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 117895481,3-Propanediol, 2-(2,2-dimethoxyethyl)-収率 66.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether
このページの内容参加物実験手順後処理出典と根拠反応ノート
溶媒

実験手順

Diethyl (2,2-dimethoxyethyl)malonate (115.0 g, 0.46 mol) was added to a suspension of lithium aluminum hydride (38.0 g, 1.00 mol) in 400 ml of dry ether at a rate to maintain a gentle reflux. After stirring for 15 min. 40 ml of water, 40 ml of 15% aqueous NaOH, and 120 ml of water were added and stirring was continued until a white suspension was obtained. The inorganic salts were filtered off and extracted with several 200 ml portions of tetrahydrofuran (THF). The combined organic extracts were evaporated and distilled twice in vacuum to yield 50.23 g (66.5%) of the title compound. B.p. 116°-125° (0.02 mm Hg).

後処理

  1. temperatureto maintain a gentle reflux
  2. stirringstirring
  3. customwas obtained
  4. filtrationThe inorganic salts were filtered off
  5. extractionextracted with several 200 ml portions of tetrahydrofuran (THF)
  6. customThe combined organic extracts were evaporated
  7. distillationdistilled twice in vacuum

出典と根拠

ORDレコード
ord-a734558324664f67a0840fe933ae2966
出典データセット
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04798833

反応ノート

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