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Acetic Anhydride → HCID 21973825、化合物

HRID 2085531
ノート
印刷プレビュー

反応式

HRID 2085531 の反応式
[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([NH:11][CH2:12][C:13]([CH3:16])([NH2:15])[CH3:14])[C:5]([CH3:17])=[C:4]([CH3:18])[N:3]=1.C(N(CC)CC)C.[C:26](OC(=O)C)(=[O:28])[CH3:27]>C(Cl)Cl>[Cl:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[C:6]([NH:11][CH2:12][C:13]([NH:15][C:26](=[O:28])[CH3:27])([CH3:14])[CH3:16])[C:5]([CH3:17])=[C:4]([CH3:18])[N:3]=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 7918Acetic AnhydrideHCID 8471TriethylamineHCID 21973832HCID 21973832、化合物

生成物 1

HCID 21973825HCID 21973825、化合物収率 83.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of gave N1-(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)-2-methylpropane-1,2-diamine (3.14 g, 10.9 mmol) in 50 mL of CH2Cl2 was cooled to 0° C. under N2 and treated with triethylamine (2.84 mL, 20.4 mmol) and acetic anhydride (1.01 mL, 10.7 mmol). After stirring for 2 h, the reaction was quenched by the addition of saturated aqueous NaHCO3. CH2Cl2 (100 mL) was added and the organic layer was separated. The organic layer was then washed with cold H2O (2×) and brine. The organic portion was dried with Na2SO4 and concentrated to give N-{2-[(2-chloro-5,6-dimethyl-3-nitropyridin-4-yl)amino]-1,1-dimethylethyl}acetamide (2.80 g) as a yellow foam.

後処理

  1. customthe reaction was quenched by the addition of saturated aqueous NaHCO3
  2. additionCH2Cl2 (100 mL) was added
  3. customthe organic layer was separated
  4. washThe organic layer was then washed with cold H2O (2×) and brine
  5. dry with materialThe organic portion was dried with Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-18885e1c10ad4bff97d609e28adffe66
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06720422B2

反応ノート

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