Acetic Anhydride → Phosphinic acid, [(benzoylamino)methyl]phenyl-

HRID 1647556ノート

反応式

HRID 1647556 の反応式
C(OC(=O)C)(=O)C.[C:8]1([P:14]([OH:16])[OH:15])[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.O[CH2:18][NH:19][C:20](=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(O)(=O)C>[C:20]([NH:19][CH2:18][P:14]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)(=[O:16])[OH:15])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 72903Phenylphosphinic acidHCID 80493N-(hydroxymethyl)benzamide

生成物 1

HCID 296994Phosphinic acid, [(benzoylamino)methyl]phenyl-収率 73%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

43.2 g (0.424 mol) of acetic anhydride were cooled to 10° C. A solution of 28.2 g (0.2 mol) of benzenephosphonous acid in 40 ml acetic acid were then added dropwise at 15° C., with stirring and cooling. After this, 30.2 g (0.2 mol) of N-hydroxymethylbenzamide were added in portions in the course of 10 minutes at 15° C., with cooling. After this, the cooling was removed, during which process the internal temperature rose to 35° C. After this, the mixture was refluxed for 3 hours and subsequently cooled. 175 ml of water were then added; during this process, the temperature rose to 35° C. The mixture was refluxed again, and finally cooled again, with stirring. After crystallisation, a total of 40 g (73% of theory) of benzoylaminomethylphenylphosphinic acid of a melting point of 158°-160° C. were obtained. CHNP analysis revealed:

後処理

  1. temperaturecooling
  2. temperaturewith cooling
  3. customAfter this, the cooling was removed, during which process the internal temperature
  4. customrose to 35° C
  5. temperatureAfter this, the mixture was refluxed for 3 hours
  6. temperaturesubsequently cooled
  7. addition175 ml of water were then added
  8. customrose to 35° C
  9. temperatureThe mixture was refluxed again
  10. temperaturefinally cooled again
  11. stirringwith stirring
  12. customAfter crystallisation

出典と根拠

ORDレコード
ord-6f88232c519d43a2a1bdfc7ba7dae6b1
出典データセット
uspto-grants-1995_07
特許番号
US05432291

反応ノート

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