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Water → 2-(Aminomethyl)-1,3-benzodioxole

HRID 1428642
ノート
印刷プレビュー

反応式

HRID 1428642 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[O:3][CH:2]1[C:10]([NH2:12])=O.[H-].[Al+3].[Li+].[H-].[H-].[H-].O>O1CCCC1>[O:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[O:3][CH:2]1[CH2:10][NH2:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 21226445Aluminium lithium hydrideHCID 57485163Benzodioxole-2-carboxamide

生成物 1

HCID 573560262-(Aminomethyl)-1,3-benzodioxole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Benzo[1,3]dioxole-2-carboxylic acid amide (5.44 g, 32.9 mmol) was dissolved in tetrahydrofuran (THF, 100 mL). Lithium aluminum hydride (LAH, 1M in THF, 39.5 mL, 39.5 mmol) was added slowly to the solution at room temperature. The reaction was stirred at room temperature for 24 hours. Distilled water was added to destroy the excess LAH. Aqueous sodium hydroxide (3.0 M, 100 mL) was added and the solution was extracted with ethyl acetate (3×100 mL). The combined organic solution was washed with water and dried over MgSO4. The solvent was evaporated to yield C-benzo[1,3]dioxol-2-yl-methylamine as a colorless oil.

後処理

  1. customto destroy the excess LAH
  2. additionAqueous sodium hydroxide (3.0 M, 100 mL) was added
  3. extractionthe solution was extracted with ethyl acetate (3×100 mL)
  4. washThe combined organic solution was washed with water
  5. dry with materialdried over MgSO4
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-abf95600aad94b74aacc98aa5a380858
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08937096B2

反応ノート

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