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

HRID 1182115
ノート
印刷プレビュー

反応式

HRID 1182115 の反応式
[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]
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 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 69357458(2-Ethyl-[1,3]dioxolan-2-yl)-acetonitrile

生成物 1

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

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

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

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

後処理

  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

出典と根拠

ORDレコード
ord-4059495ffebc446bbaf2a7eb39ac22a3
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07288537B2

反応ノート

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