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Ethyl Acetate → Acetic acid 2-(6-aminomethyl-2-nitropyridin-3-yloxy)-ethyl ester

HRID 15013
ノート
印刷プレビュー

反応式

HRID 15013 の反応式
O=C1C2C(=CC=CC=2)C(=O)[N:3]1[CH2:12][C:13]1[N:18]=[C:17]([N+:19]([O-:21])=[O:20])[C:16]([O:22][CH2:23][CH2:24][O:25][C:26](=[O:28])[CH3:27])=[CH:15][CH:14]=1.O.NN.C(OCC)(=O)C>C(O)C>[NH2:3][CH2:12][C:13]1[N:18]=[C:17]([N+:19]([O-:21])=[O:20])[C:16]([O:22][CH2:23][CH2:24][O:25][C:26](=[O:28])[CH3:27])=[CH:15][CH:14]=1
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 8857Ethyl AcetateHCID 24654Hydrazine hydrate (1:1)HCID 59341198Acetic acid 2-[6-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-nitro-pyridin-3-yloxy]-ethyl ester

生成物 1

HCID 59341182Acetic acid 2-(6-aminomethyl-2-nitropyridin-3-yloxy)-ethyl ester

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 0.35 gm (0.97 mmol) of Acetic acid 2-[6-(1,3-dioxo-1,3-dihydro-isoindol-2-ylmethyl)-nitro-pyridin-3-yloxy]-ethyl ester 97 in 5 mL of ethanol was added 0.051 mL (1.01 mmol) of hydrazine hydrate at room temperature. The reaction mixture was allowed to stir for 4 h. The mixture was then transferred with ethyl acetate and the solvent was removed at reduced pressure. The residue was taken up in CHCl3 (200 mL) and washed twice with water (100 mL), saturated brine, dried (Na2SO4), and the solvents removed under reduced pressure. This was used without further purification or characterization.

後処理

  1. customthe solvent was removed at reduced pressure
  2. washwashed twice with water (100 mL), saturated brine
  3. dry with materialdried (Na2SO4)
  4. customthe solvents removed under reduced pressure
  5. customThis was used without further purification or characterization

出典と根拠

ORDレコード
ord-161543088d4b45fdbc2f9dfd4438b41e
出典データセット
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07732457B2

反応ノート

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