Bromotrimethylsilane → Phosphonic acid, P-(3-aminophenyl)-

HRID 705452

反応式

HRID 705452 の反応式
C[Si](Br)(C)C.C[O:7][P:8]([C:11]1[CH:16]=[CH:15][CH:14]=[C:13]([N+:17]([O-])=O)[CH:12]=1)(=[O:10])[O-:9]>CN(C=O)C>[NH2:17][C:13]1[CH:12]=[C:11]([P:8](=[O:7])([OH:10])[OH:9])[CH:16]=[CH:15][CH:14]=1

参加物

4

反応物 2

HCID 76113BromotrimethylsilaneHCID 117629312HCID 117629312、化合物

生成物 1

HCID 79477Phosphonic acid, P-(3-aminophenyl)-

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

4 mL of DMF and trimethylsilyl bromide (1 mL) were added to the mixture (170 mg) of monomethyl(3-nitrophenyl)phosphonate and dimethyl ester, and stirred at 60° C. for 2 hours. After removing a solvent, the mixture was dissolved in a mixed solvent of water and methanol. Pd/C in catalyst quantity was added thereto and stirred under hydrogen atmosphere overnight. After filtering out the catalyst, a solvent was removed to obtain a crude product of (3-aminophenyl)phosphonic acid.

後処理

  1. customAfter removing a solvent
  2. dissolutionthe mixture was dissolved in a mixed solvent of water and methanol
  3. additionPd/C in catalyst quantity was added
  4. stirringstirred under hydrogen atmosphere overnight
  5. filtrationAfter filtering out the catalyst
  6. customa solvent was removed

出典と根拠

ORDレコード
ord-6a63d25663584b4a98789a2ec6aac73f
出典データセット
uspto-grants-2015_11
特許番号
US09174932B2

関連ノート

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