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Methanol → 2-(3-Chloro-4-fluorophenyl)ethan-1-amine hydrochloride

HRID 639522
ノート
印刷プレビュー

反応式

HRID 639522 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][C:10]#[N:11])[CH:5]=[CH:6][C:7]=1[F:8].CO>C1COCC1>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH2:9][CH2:10][NH2:11])[CH:5]=[CH:6][C:7]=1[F:8]
参加物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 887MethanolHCID 27737253-Chloro-4-fluorobenzyl cyanide

生成物 1

HCID 685761312-(3-Chloro-4-fluorophenyl)ethan-1-amine hydrochloride収率 145%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Borane-tetrahydrofuran complex solution (1 M in THF, 132 mL, 132 mmol) was added dropwise over 30 min at 0-5° C. to a solution of 3-chloro-4-fluoro-phenylacetonitrile (4.37 g, 25.8 mmol) in THF (40 mL), then the reaction mixture was stirred at RT for 20 min and refluxed for 21 h. The reaction mixture was then cooled to 0° C., and methanol (30 mL) was added at 2-5° C. over 45 minutes. After refluxing for 1 h the reaction mixture was concentrated, the residue dissolved in dichloromethane and the amine extracted twice with 1 M aq. hydrochloric acid solution. The combined aqueous phases were then treated with concentrated aq. sodium hydroxide solution to adjust the pH to 12, then extracted twice with dichloromethane. The combined organic phases were washed with water, dried over magnesium sulfate, filtered and concentrated, leading to a colorless oil (4.3 g). This was dissolved in diethyl ether (125 mL), treated with hydrogen chloride solution (2.6 M in diethyl ether), and stirred at RT for 1 h. The precipitate was then collected by filtration to afford the title compound (3.93 g, 73%) White solid, MS (ISP) 174.1 (M−Cl)+.

後処理

  1. temperaturerefluxed for 21 h
  2. temperatureThe reaction mixture was then cooled to 0° C.
  3. temperatureAfter refluxing for 1 h the reaction mixture
  4. concentrationwas concentrated
  5. dissolutionthe residue dissolved in dichloromethane
  6. extractionthe amine extracted twice with 1 M aq. hydrochloric acid solution
  7. additionThe combined aqueous phases were then treated with concentrated aq. sodium hydroxide solution
  8. extractionextracted twice with dichloromethane
  9. washThe combined organic phases were washed with water
  10. dry with materialdried over magnesium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. dissolutionThis was dissolved in diethyl ether (125 mL)
  14. additiontreated with hydrogen chloride solution (2.6 M in diethyl ether)
  15. stirringstirred at RT for 1 h
  16. filtrationThe precipitate was then collected by filtration

出典と根拠

ORDレコード
ord-c12ddce50e8c405e9076d479b13f0026
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691876B2

反応ノート

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