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Triethylamine → Neodymium

HRID 1710305
ノート
印刷プレビュー

反応式

HRID 1710305 の反応式
[O:1]([CH2:8][CH2:9][C:10]1[CH:18]=[CH:17][CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]=1[C:19]([OH:21])=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.[N+]([O-])([O-])=O.[Nd+3:33].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>C(O)C>[Nd:33].[O:1]([CH2:8][CH2:9][C:10]1[CH:18]=[CH:17][CH:16]=[C:12]([C:13]([OH:15])=[O:14])[C:11]=1[C:19]([OH:21])=[O:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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

6

反応物 3

HCID 8471Triethylamine2 回HCID 10980413Neodymium(3+) hydrate trinitrate2 回HCID 68740870Mono(2-phenoxyethyl)phthalic acid2 回

生成物 2

HCID 23934NeodymiumHCID 68740870Mono(2-phenoxyethyl)phthalic acid

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒
4 回

反応条件

温度
40 °C

実験手順

The mono(2-phenoxyethyl)phthalic acid obtained in 6-1 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 88.6 g of the mono(2-phenoxyethyl)phthalic acid obtained in 6-1, 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(2-phenoxyethyl)phthalic acid-triethylamine salts. 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 2 hours, to produce a synthesis solution of a neodymium salt of mono(2-phenoxyethyl)phthalic acid. Then, ethanol was distilled from this synthesis solution to concentrate, 300 ml of dichloromethane were added to the concentrate to form a solution, this solution was transferred to a 1 L separating funnel, shaken after pouring 400 ml of water into this separating funnel, and the resulting neodymium salts of mono(2-phenoxyethyl)phthalic acid were washed. After further washing this dichloromethane solution twice with 400 ml of water, the dichloromethane was distilled out. The solid obtained by distillation was crushed, then dried under reduced pressure at 50° C. to obtain 94.0 g of a neodymium salt of mono(2-phenoxyethyl)phthalic acid (yield 94%).

後処理

  1. customa reactor similar to the above was used
  2. stirringto stir a solution
  3. customobtained
  4. customobtained in 6-1
  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. dissolutionby dissolving
  10. stirringwhile stirring
  11. temperaturethe solution was heated to 40° C. for 2 hours

出典と根拠

ORDレコード
ord-2a6000f4362f469faa5f484971395794
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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