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Triethylamine → Neodymium

HRID 1710301
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HRID 1710301 반응식
[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])[CH:2]([CH3:4])[CH3:3].C(N(CC)CC)C.[N+]([O-])([O-])=O.[Nd+3:28].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>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])[CH:2]([CH3:4])[CH3:3]
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6

반응물 3

HCID 8471Triethylamine2회HCID 10980413Neodymium(3+) hydrate trinitrate2회HCID 22394963Monoisobutylphthalic Acid2회

생성물 2

HCID 23934NeodymiumHCID 22394963Monoisobutylphthalic Acid

시약·촉매·용매 1

HCID 702Ethanol
용매
4회

반응 조건

온도
20 °C

실험 절차

The monoisobutylphthalic acid obtained in 1-1 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 that of 1-1 was used to stir a solution obtained by adding 30 ml of an anhydrous ethanol to 70.0 g of the monoisobutylphthalic acid obtained in 1-1, while dripping 30.4 g of triethylamine while maintaining at 20° C. 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 monoisobutylphthalic 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 30 minutes, to produce a synthesis solution of a neodymium salt of monoisobutylphthalic 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 monoisobutylphthalic acid was extracted and washed. After further washing this chloroform solution with water twice, it was transferred to a 2 L cylindrical separable flask, and 800 ml of hexane were slowly added while stirring to crystallize. Crystals obtained by filtering this slurry solution, then further the filtered crystals were added to 400 ml of hexane, stirred and washed, then refiltered, and the crystals were dried under reduced pressure at 50° C., to obtain 68.1 g of a neodymium salt of monoisobutylphthalic acid (yield 84%).

후처리

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

출처 및 근거

ORD 기록
ord-b8b43f53f80543279df9c954e3a0276b
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790290B2

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