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Ethylamine → Ethyl(3-(3-pyridyloxy)propyl)amine

HRID 2305722
ノート
印刷プレビュー

反応式

HRID 2305722 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.[CH2:12]([NH2:14])[CH3:13]>CO.O1CCCC1>[CH2:12]([NH:14][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)[CH3:13]
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

5

反応物 2

HCID 6341EthylamineHCID 184333433-(3-Chloro-propoxy)-pyridine

生成物 1

HCID 9877539Ethyl(3-(3-pyridyloxy)propyl)amine収率 38.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
100 °C

実験手順

The 3-chloro-1-(3-pyridyloxy)propane (1.00 g, 5.84 mmol) was dissolved in methanol (50 mL) and added to a 2.0 M solution of ethylamine in tetrahydrofuran (5 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 impurities were extracted with ether (3×15 mL). The aqueous layer was basified to pH 10 with 10% NaOH solution and extracted with chloroform (4×15 mL). The combined chloroform extracts were dried (Na2SO4), filtered, and concentrated by rotary evaporation to a residue that was dried briefly under high vacuum to give 400 mg (38.1%) 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. extractionwere extracted with ether (3×15 mL)
  6. extractionextracted with chloroform (4×15 mL)
  7. dry with materialThe combined chloroform extracts were dried (Na2SO4)
  8. filtrationfiltered
  9. concentrationconcentrated by rotary evaporation to a residue that
  10. customwas dried briefly under high vacuum

出典と根拠

ORDレコード
ord-d9eafff77a844611aa285e57205dc0a6
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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