Potassium Iodide → N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamine

HRID 442714

反応式

HRID 442714 の反応式
Cl.Cl[CH2:3][CH2:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1.[CH3:11][N:12]([CH3:15])[CH2:13][NH2:14].[C:16](=O)(O)[O-].[Na+].[I-].[K+]>C(O)C>[CH3:11][N:12]([CH3:15])[CH:13]([NH:14][CH2:3][CH2:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1)[CH3:16]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 199465Pyridine, 3-(2-chloroethyl)-, hydrochlorideHCID 516892Sodium BicarbonateHCID 5250464Methanediamine, N,N-dimethyl-

生成物 1

HCID 18788472N,N-dimethyl N'-[2-(3-pyridyl)ethyl]ethanediamine収率 56.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

11 g of 3-(2-chloroethyl)pyridine hydrochloride, 16.3 g of N,N-dimethylmethane diamine, 18.5 g of sodium bicarbonate and 13 g of potassium iodide are heated in 150 ml of ethanol for about 30 hours at about 60° C. The solvent is evaporated and the residue is taken up in 100 ml of water before an aqueous solution of 10N NaOH is added to give pH 8; the aqueous phase is then extracted 3 times with 80 ml of ethyl acetate. The pooled organic phases are dried over magnesium sulfate, filtered and concentrated under reduced pressure. The residual oil is distilled to give 6.7 g of the expected product. B.p.=100°-107° C./10 Pa.

後処理

  1. customThe solvent is evaporated
  2. additionis added
  3. customto give pH 8
  4. extractionthe aqueous phase is then extracted 3 times with 80 ml of ethyl acetate
  5. dry with materialThe pooled organic phases are dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. distillationThe residual oil is distilled

出典と根拠

ORDレコード
ord-d05e5e98888c4387ad6e9e5349237657
出典データセット
uspto-grants-1999_04
特許番号
US05891893

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