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

HRID 614365

反応式

HRID 614365 の反応式
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

参加物

3

反応物 2

HCID 3301EthylenediamineHCID 881004-Bromopyridinium chloride

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5b5683f49b9c4128b6fd1fc128486bcb
出典データセット
uspto-grants-1979_03
特許番号
US04144344

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