Ethylenediamine → N1-(pyridin-4-yl)ethane-1,2-diamine

HRID 614365

반응식

HRID 614365 반응식
Cl.Br[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.[CH2:9]([NH2:12])[CH2:10][NH2:11]>>[NH2:11][CH2:10][CH2:9][NH:12][C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1

참가 물질

3

반응물 2

HCID 3301EthylenediamineHCID 881004-Bromopyridinium chloride

생성물 1

HCID 14834209N1-(pyridin-4-yl)ethane-1,2-diamine

실험 절차

A mixture of 38.9 g of 4-bromo-pyridine-hydrochloride and 480 g of ethylenediamine is refluxed with stirring for 13 hours. The reaction mixture is thereafter concentrated under reduced pressure and the residue is treated with toluene and concentrated once more. The residue is made alkaline with a concentrated aqueous solution of sodium hydroxide and extracted with five 75 ml portions of methylene chloride. The combined extracts are dried over sodium sulphate and concentrated under reduced pressure. Recrystallisation of the residue from methylene chloride yields 4-(2-aminoethylamino)-pyridine as a light yellow crystalline substance with a melting point of 120°-121° C.

후처리

  1. temperatureis refluxed
  2. concentrationThe reaction mixture is thereafter concentrated under reduced pressure
  3. additionthe residue is treated with toluene
  4. concentrationconcentrated once more
  5. extractionextracted with five 75 ml portions of methylene chloride
  6. dry with materialThe combined extracts are dried over sodium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customRecrystallisation of the residue from methylene chloride

출처 및 근거

ORD 기록
ord-5b5683f49b9c4128b6fd1fc128486bcb
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144344

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