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Acetic Anhydride → Sodium

HRID 437095
ノート
印刷プレビュー

反応式

HRID 437095 の反応式
[Na:1].[NH2:2][C:3]([P:9]([OH:12])(=[O:11])[OH:10])([P:5]([OH:8])(=[O:7])[OH:6])[CH3:4].[C:13](OC(=O)C)(=[O:15])[CH3:14]>O>[Na:1].[C:13]([NH:2][C:3]([P:5]([OH:8])(=[O:6])[OH:7])([P:9]([OH:12])(=[O:10])[OH:11])[CH3:4])(=[O:15])[CH3:14]
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 3

HCID 7918Acetic AnhydrideHCID 84770(1-Aminoethylidene)bisphosphonic acidHCID 5360545Sodium

生成物 2

HCID 5360545SodiumHCID 22155105Phosphonic acid, [1-(acetylamino)ethylidene]bis-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

22.7 g. (0.1 mole) of the mono-sodium salt of 1-amino ethane-1,1-diphosphonic acid are boiled under reflux in 30.6 g. (0.3 moles) of acetic acid anhydride for about 30 minutes. A clear solution is obtained. On cooling, a viscous yellowish sirup is produced. The sirup can be diluted with water and the aqueous solution can be used directly. In order to recover the crystalline reaction product, the sirup is added with stirring to 40 cc. of glacial acetic acid and the resulting crystalline product is filtered off by suction. After drying, 20.3 g. of the mono-sodium salt of N-acetyl-1-amino ethane-1,1-diphosphonic acid, corresponding to 75.4 % of the theoretical yield, are obtained.

後処理

  1. temperatureunder reflux in 30.6 g
  2. customA clear solution is obtained
  3. temperatureOn cooling
  4. customa viscous yellowish sirup is produced
  5. customIn order to recover the crystalline reaction product
  6. additionthe sirup is added
  7. filtrationof glacial acetic acid and the resulting crystalline product is filtered off by suction
  8. customAfter drying

出典と根拠

ORDレコード
ord-43e8e1ab3e064ea3a83b2411ef5b8b23
出典データセット
uspto-grants-1977_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04029697

反応ノート

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