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

HRID 129810

反応式

HRID 129810 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]([CH3:16])[CH:13]([NH2:15])[CH3:14].C(=O)(O)[O-].[Na+].[I-].[K+]>C(O)C>[CH3:11][N:12]([CH3:16])[CH:13]([NH:15][CH2:3][CH2:4][C:5]1[CH:6]=[N:7][CH:8]=[CH:9][CH:10]=1)[CH3:14]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 199465Pyridine, 3-(2-chloroethyl)-, hydrochlorideHCID 516892Sodium BicarbonateHCID 18943179N~1~,N~1~-Dimethylethane-1,1-diamine

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-dimethylethane 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.

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-90c7c5d20a114624b6aae3318d1b3f37
出典データセット
uspto-grants-1995_11
特許番号
US05470855

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