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Water → tert-Butyl 2-(2-nitrophenylamino)ethylcarbamate

HRID 2267285
ノート
印刷プレビュー

反応式

HRID 2267285 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[NH2:11][CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18].C(N(CC)CC)C.O>O1CCCC1>[N+:8]([C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[NH:11][CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:19])([CH3:18])[CH3:20])([O-:10])=[O:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 738951-Fluoro-2-nitrobenzeneHCID 187201N-BOC-ethylenediamine

生成物 1

HCID 47453724tert-Butyl 2-(2-nitrophenylamino)ethylcarbamate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 1-fluoro-2-nitrobenzene (2 g, 14.2 mmol), tert-butyl 2-aminoethylcarbamate (2.7 g, 17.0 mmol) and triethylamine (1.7 g, 2.4 mmol) in tetrahydrofuran was refluxed for 7 h. After cooling to rt 100 mL of water was added and the mixture was extracted with ethyl acetate (3×100 mL). The combined organic layer was washed with brine (150 mL), dried over anhydrous sodium sulfate and filtered. The solvent was removed and the product was used in the next step without further purification.

後処理

  1. temperaturewas refluxed for 7 h
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate (3×100 mL)
  4. washThe combined organic layer was washed with brine (150 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. customThe solvent was removed
  8. customthe product was used in the next step without further purification

出典と根拠

ORDレコード
ord-366af49cab344e688837a679a5878da8
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858785B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート