Acetic Anhydride → HCID 20559958, 화합물

HRID 1579335노트

반응식

HRID 1579335 반응식
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]

참가 물질

4

반응물 2

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

생성물 1

HCID 20559958HCID 20559958, 화합물수율 83%

시약·촉매·용매 1

HCID 284Formic Acid용매

반응 조건

온도
25 °C

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-bef9b1ad628245b2819782ff7bf6efc7
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03931195

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