Acetic Anhydride → HCID 20559958、化合物

HRID 1579335ノート

反応式

HRID 1579335 の反応式
C(O[C:5](=[O:7])C)(=O)C.[NH2:8][C:9]1[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=1[CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1>C(O)=O>[CH:5]([NH:8][C:9]1[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=1[CH2:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=1)=[O:7]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 47154222-(2-(Pyridin-2-YL)ethyl)aniline

生成物 1

HCID 20559958HCID 20559958、化合物収率 83%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

反応条件

温度
25 °C

実験手順

An aceticformic anhydride mixture is prepared by mixing acetic anhydride (140 ml.) and formic acid (70 ml.). To this mixture, 2-(o-aminophenethyl)pyridine (59 g., 0.3 mole) is added in one portion with vigorous stirring at 25°C. After 15 minutes the solution is diluted with 450 ml. of water and concentrated in vacuo. The resulting residue is taken up in 1 liter of water and made basic with 50% sodium hydroxide. The basified solution is extracted with chloroform, the chloroform extract washed with water, dried over magnesium sulfate and the chloroform solvent evaporated. Crystallization of the residue from isopropyl acetate provides 57 g. (83% yield) of 2-(o-formamidophenethyl)pyridine melting at 78°-81°C. (uncorrected). An analytical sample (from isopropyl acetate) has a melting point of 83°-83.5°C. (corr.).

後処理

  1. additionAfter 15 minutes the solution is diluted with 450 ml
  2. concentrationof water and concentrated in vacuo
  3. extractionThe basified solution is extracted with chloroform
  4. extractionthe chloroform extract
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. customthe chloroform solvent evaporated
  8. customCrystallization of the residue from isopropyl acetate
  9. customprovides 57 g

出典と根拠

ORDレコード
ord-bef9b1ad628245b2819782ff7bf6efc7
出典データセット
uspto-grants-1976_01
特許番号
US03931195

反応ノート

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