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

HRID 533434
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HRID 533434 반응식
[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]
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참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-83ff7945785e4b449e765e00c7239ac6
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08853263B2

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