Acetic Anhydride → HCID 20030813, 화합물

HRID 232033노트

반응식

HRID 232033 반응식
[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]

참가 물질

3

반응물 2

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

생성물 1

HCID 20030813HCID 20030813, 화합물수율 59%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1dfb6fb7964942569b1237c1c3df3738
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851412

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