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Formic Acid → N-formyl-2-amino-3',5-di-t-butyl biphenyl

HRID 338193
ノート
印刷プレビュー

反応式

HRID 338193 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:4][C:3]=1[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:13]=1.[CH:22](O)=[O:23]>O>[CH:22]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([CH3:9])([CH3:10])[CH3:11])=[CH:4][C:3]=1[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([CH3:21])([CH3:20])[CH3:19])[CH:13]=1)=[O:23]
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 284Formic AcidHCID 66813837HCID 66813837、化合物

生成物 1

HCID 86614227N-formyl-2-amino-3',5-di-t-butyl biphenyl収率 82%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Added 2-amino-3′,5-di-t-butyl biphenyl (2.0 g, 7.11 mmol) to a solution of formic acid and heated to reflux for 16 hours. After cooling, water (25 mL) was added the product and the precipitate collected by vacuum filtration. The crude product was dissolved into ethyl acetate, washed with water. The organics were dried over magnesium sulfate and concentrated and purified by column chromatography using 10% ethyl acetate and hexanes as the eluants to give the pure N-formyl-2-amino-3′,5-di-t-butyl biphenyl (1.8 g, 82% yield) as determined by GCMS.

後処理

  1. temperatureheated
  2. temperatureto reflux for 16 hours
  3. temperatureAfter cooling
  4. filtrationthe precipitate collected by vacuum filtration
  5. dissolutionThe crude product was dissolved into ethyl acetate
  6. washwashed with water
  7. dry with materialThe organics were dried over magnesium sulfate
  8. concentrationconcentrated
  9. custompurified by column chromatography

出典と根拠

ORDレコード
ord-7bfb07ec342945e6935e5c954aaf41de
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08889864B2

反応ノート

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