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Dimethylamine → Dimethyl(3-(3-pyridyloxy)propyl)amine

HRID 2305697
ノート
印刷プレビュー

反応式

HRID 2305697 の反応式
Cl[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1.[CH3:12][NH:13][CH3:14]>CO>[CH3:12][N:13]([CH3:14])[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 674DimethylamineHCID 184333433-(3-Chloro-propoxy)-pyridine

生成物 1

HCID 9794053Dimethyl(3-(3-pyridyloxy)propyl)amine収率 92.9%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

The 3-chloro-1-(3-pyridyloxy)propane (2.00 g, 11.65 mmol) was dissolved in methanol (25 mL) and added to a 40 wt % aqueous solution of dimethylamine (50 mL) in a heavy-walled glass pressure-tube apparatus. The tube was sealed and the mixture was stirred and heated at 100° C. (oil bath temperature) for 4 h. After cooling, the mixture was concentrated by rotary evaporation. Saturated NaCl solution (25 mL) was added to the residue. The pH of the solution was adjusted to 6, and the mixture was extracted with ether (3×25 mL) to remove impurities. The aqueous layer was basified to pH 10 with 10% NaOH solution and extracted with chloroform (4×50 mL). The combined chloroform extracts were dried (Na2SO4), filtered, and concentrated to give 1.95 g (92.9%) of an oil.

後処理

  1. customThe tube was sealed
  2. temperatureAfter cooling
  3. concentrationthe mixture was concentrated by rotary evaporation
  4. additionSaturated NaCl solution (25 mL) was added to the residue
  5. extractionthe mixture was extracted with ether (3×25 mL)
  6. customto remove impurities
  7. extractionextracted with chloroform (4×50 mL)
  8. dry with materialThe combined chloroform extracts were dried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-0c8a300fc684477c9bfaed0c76cb5716
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06441006B2

反応ノート

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