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Triethylamine → Neodymium

HRID 1710303
ノート
印刷プレビュー

反応式

HRID 1710303 の反応式
[CH2:1]([C:5]1[CH:13]=[CH:12][CH:11]=[C:7]([C:8]([OH:10])=[O:9])[C:6]=1[C:14]([OH:16])=[O:15])[CH2:2][CH2:3][CH3:4].C(N(CC)CC)C.[N+]([O-])([O-])=O.[Nd+3:28].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.C(N(CC)CC)C.C(C1C=CC=C(C(O)=O)C=1C(O)=O)CCC>C(O)C>[Nd:28].[CH2:1]([C:5]1[CH:13]=[CH:12][CH:11]=[C:7]([C:8]([OH:10])=[O:9])[C:6]=1[C:14]([OH:16])=[O:15])[CH2:2][CH2:3][CH3:4]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8471Triethylamine2 回HCID 10980413Neodymium(3+) hydrate trinitrate2 回HCID 139815183-Butylphthalic acid2 回HCID 68741096Mono-n-butylphthalic acid-triethylamine salt

生成物 2

HCID 23934NeodymiumHCID 139815183-Butylphthalic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒4 回

反応条件

温度
40 °C

実験手順

The mono-n-butylphthalic acid obtained in 5-1 was formed into a triethylamine salt in anhydrous ethanol, after which an ethanol solution of neodymium nitrate was added while stirring. That is, a reactor similar to the above was used to stir a solution obtained by adding 30 ml of an anhydrous ethanol to 68.1 g of the mono-n-butylphthalic acid obtained in 5-1, while dripping 30.4 g of triethylamine while maintaining at 30° C. or less by cooling in an ice water bath. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a synthesis solution of mono-n-butylphthalic acid-triethylamine salt. Next, this synthesis solution was adjusted to 20° C., and a solution obtained by dissolving 43.8 g of neodymium nitrate into 100 ml of ethanol was dripped in while stirring. After dripping, the solution was heated to 40° C. for 30 minutes, to produce a synthesis solution of a neodymium salt of mono-n-butylphthalic acid. Then, ethanol was distilled from this synthesis solution to concentrate, 150 ml of chloroform and 200 ml of water were added to the concentrate and stirred, and the resulting neodymium salt of mono-n-butylphthalic acid was extracted and washed. After further washing this chloroform solution with, water twice, the chloroform was distilled out. The solid obtained by distillation was crushed, then dried under reduced pressure at 50° C. to obtain 72.9 g of a neodymium salt of mono-n-butylphthalic acid (yield 90%).

後処理

  1. customa reactor similar to the above was used
  2. stirringto stir a solution
  3. customobtained
  4. customobtained in 5-1
  5. temperaturewhile maintaining at 30° C. or less
  6. temperatureby cooling in an ice water bath
  7. customwas adjusted to 20° C.
  8. customa solution obtained
  9. stirringwhile stirring
  10. temperaturethe solution was heated to 40° C. for 30 minutes

出典と根拠

ORDレコード
ord-3f502ade04384591b6203b31e27cdd69
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07790290B2

反応ノート

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