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Sodium Hydroxide → 2-(4-Bromo-2-nitrophenyl)ethan-1-amine

HRID 1793941
ノート
印刷プレビュー

反応式

HRID 1793941 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][NH:10]C(=O)C(F)(F)F)=[C:4]([N+:17]([O-:19])=[O:18])[CH:3]=1.[OH-].[Na+]>CO>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][NH2:10])=[C:4]([N+:17]([O-:19])=[O:18])[CH:3]=1
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 14798Sodium HydroxideHCID 22219483HCID 22219483、化合物

生成物 1

HCID 222194872-(4-Bromo-2-nitrophenyl)ethan-1-amine収率 98.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 4.856 g of N-[2-(4-bromo-2-nitrophenyl)ethyl]-2,2,2-trifluoroacetamide in 56 mL of methanol was added 3.417 mL of 5 mol/L sodium hydroxide solution. After being stirred at room temperature overnight, and at 50° C. overnight, the reaction mixture was concentrated under reduced pressure. To the residue were added ethyl acetate and water, and the mixture was separated. After the aqueous layer was extracted with ethyl acetate, the organic layers were combined, and washed with brine. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was removed under reduced pressure to give 3.44 g of 2-(4-bromo-2-nitrophenyl)ethylamine.

後処理

  1. concentrationat 50° C. overnight, the reaction mixture was concentrated under reduced pressure
  2. additionTo the residue were added ethyl acetate and water
  3. customthe mixture was separated
  4. extractionAfter the aqueous layer was extracted with ethyl acetate
  5. washwashed with brine
  6. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-1d651983b4d24b16a8a786fbe1590a8e
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07022689B2

反応ノート

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