Benzo-1,3-dioxole-5-acetic acid → 2-(1,3-Dioxaindan-5-yl)ethan-1-ol

HRID 375576ノート

反応式

HRID 375576 の反応式
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11](O)=[O:12])=[CH:4][C:3]=2[O:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>CCOCC>[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][CH2:11][OH:12])=[CH:4][C:3]=2[O:2]1

参加物

4

反応物 2

HCID 76115Benzo-1,3-dioxole-5-acetic acidHCID 21226445Aluminium lithium hydride

生成物 1

HCID 27598462-(1,3-Dioxaindan-5-yl)ethan-1-ol収率 90.4%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

3,4-Methylenedioxyphenylacetic acid (18.0 g) was added portionwise over 30 minutes to a stirred, ice-cooled suspension of lithium aluminium hydride (4.0 g) in ether (400 ml) and the mixture was stirred at room temperature for two hours, quenched by the cautious addition of saturated aqueous ammonium chloride solution and filtered. The filtrate was washed with 10% aqueous sodium carbonate solution, dried over magnesium sulphate and evaporated to give the title compound as a pale yellow oil (15.01 g, 90%), which was characterised by its 1H-NMR spectrum.

後処理

  1. temperaturecooled
  2. customquenched by the cautious addition of saturated aqueous ammonium chloride solution
  3. filtrationfiltered
  4. washThe filtrate was washed with 10% aqueous sodium carbonate solution
  5. dry with materialdried over magnesium sulphate
  6. customevaporated

出典と根拠

ORDレコード
ord-745dc2ab3062421ab362e02db49ab10b
出典データセット
uspto-grants-1996_01
特許番号
US05486527

反応ノート

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