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Sodium Hydroxide → 2-(2-Ethyl [1,3]dioxolan-2-yl)-N-hydroxy-acetamidine

HRID 1182115
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HRID 1182115 반응식
[OH-:1].[Na+].Cl.[NH2:4]O.[CH2:6]([C:8]1([CH2:13][C:14]#[N:15])[O:12][CH2:11][CH2:10][O:9]1)[CH3:7]>O.CO>[CH2:6]([C:8]1([CH2:13][C:14]([NH:4][OH:1])=[NH:15])[O:12][CH2:11][CH2:10][O:9]1)[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 69357458(2-Ethyl-[1,3]dioxolan-2-yl)-acetonitrile

생성물 1

HCID 1784368352-(2-Ethyl [1,3]dioxolan-2-yl)-N-hydroxy-acetamidine

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

A solution of NaOH (1.17 g, 29.3 mmol) in water/methanol (1:1) (18 ml), cooled to 0° C. in an ice bath, is treated with hydroxylamine hydrochloride (1.58 g, 22.78 mmol), with stirring for 5 minutes. (2-Ethyl-[1,3]dioxolan-2-yl)-acetonitrile (1.42 g, 10.125 mmol) is added and the reaction mixture stirred at room temperature for 18 hours, then refluxed for a further 2 hours. The reaction mixture is cooled and partitioned between ethyl acetate and water. The organic phase is dried over MgSO4, filtered, and the solvent evaporated to yield 2-(2-Ethyl [1,3]dioxolan-2-yl)-N-hydroxy-acetamidine. [M+H] 175.21

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후처리

  1. stirringthe reaction mixture stirred at room temperature for 18 hours
  2. temperaturerefluxed for a further 2 hours
  3. temperatureThe reaction mixture is cooled
  4. custompartitioned between ethyl acetate and water
  5. dry with materialThe organic phase is dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-4059495ffebc446bbaf2a7eb39ac22a3
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07288537B2

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