Acetic Anhydride → HCID 20030813、化合物

HRID 232033ノート

反応式

HRID 232033 の反応式
[OH:1][CH2:2][CH2:3][NH:4][C:5]1[C:10]([NH2:11])=[CH:9][CH:8]=[CH:7][N:6]=1.[C:12](OC(=O)C)(=O)[CH3:13]>>[OH:1][CH2:2][CH2:3][N:4]1[C:5]2=[N:6][CH:7]=[CH:8][CH:9]=[C:10]2[N:11]=[C:12]1[CH3:13]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 157187622-[(3-Aminopyridin-2-yl)amino]ethan-1-ol

生成物 1

HCID 20030813HCID 20030813、化合物収率 59%

実験手順

2-(2-Hydroxyethylamino)-3-aminopyridine (3.4 g) was dissolved in acetic anhydride (140 ml) and stirred at reflux for 15 hours. The reaction mixture was cooled and the excess of reagent removed under reduced pressure. The dark brown oil was dissolved in ethanol (100 ml), 2N sodium hydroxide (50 ml) was added and the mixture was stirred for 15 minutes. The solution was acidified to pH5 using 2N hydrochloric acid and the solvents removed under reduced pressure. The residue was chromatographed over silica eluting with 10% methanol in ethyl acetate to yield the title compound (2.32 g, 59%) as a foam.

後処理

  1. temperatureat reflux for 15 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe excess of reagent removed under reduced pressure
  4. dissolutionThe dark brown oil was dissolved in ethanol (100 ml)
  5. addition2N sodium hydroxide (50 ml) was added
  6. stirringthe mixture was stirred for 15 minutes
  7. customthe solvents removed under reduced pressure
  8. customThe residue was chromatographed over silica eluting with 10% methanol in ethyl acetate

出典と根拠

ORDレコード
ord-1dfb6fb7964942569b1237c1c3df3738
出典データセット
uspto-grants-1989_07
特許番号
US04851412

反応ノート

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