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Triethylamine → 2-Methoxybenzoic acid

HRID 1710308
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HRID 1710308 반응식
[N+]([O-])([O-])=O.[Nd+3:5].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[CH3:14][O:15][C:16]1[CH:24]=[CH:23][CH:22]=[CH:21][C:17]=1[C:18]([OH:20])=[O:19].C(N(CC)CC)C>C(O)C>[Nd:5].[CH3:14][O:15][C:16]1[CH:24]=[CH:23][CH:22]=[CH:21][C:17]=1[C:18]([OH:20])=[O:19]
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참가 물질

6

반응물 3

HCID 8471Triethylamine2회HCID 113702-Methoxybenzoic acidHCID 10980413Neodymium(3+) hydrate trinitrate2회

생성물 2

HCID 113702-Methoxybenzoic acid수율 85%HCID 23934Neodymium

시약·촉매·용매 1

HCID 702Ethanol용매
4회

반응 조건

온도
25 °C

실험 절차

The compound was synthesized by the same method as that for Synthesis Example 1-2 above, that is, after forming a triethylamine salt of 2-methoxybenzoic acid in anhydrous ethanol, an ethanol solution of neodymium nitrate was added while stirring. Specifically, a reactor similar to that of 1-1 was used to stir a slurry solution obtained by adding 100 ml of an anhydrous ethanol to 45.65 g (0.3 mol) of 2-methoxybenzoic acid, while dripping 30.4 g (0.3 mol) of triethylamine while maintaining at 20-30° C. by cooling in an ice water bath. After dripping about one-third of the triethylamine, the slurry disappeared and became transparent. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a transparent synthesis solution of 2-methoxybenzoic acid-triethylamine salts. Next, while stirring this synthesis solution and holding at 25° C., a solution obtained by dissolving 43.8 g of neodymium nitrate into 120 ml of ethanol was dripped in. Upon completion of dripping, the solution was heated to 40° C., began to cloud after 40 minutes, and the clouding increased with time. After another 20 minutes, it became an extremely thick slurry solution, so 100 ml of ethanol were further added, and the solution was stirred for another hour at 40° C., then cooled to end the reaction. Next, crystals obtained by filtering this slurry solution were added to 200 ml of methanol, stirred and washed, then refiltered, and 200 ml of methanol were once again added to the crystals, stirred and washed, then filtered. The resulting crystals were dried under reduced pressure at 50° C., to obtain 50.83 g of a neodymium salt of 2-methoxybenzoic acid (yield 85%).

후처리

  1. customSpecifically, a reactor similar to that of 1-1 was used
  2. stirringto stir a slurry solution
  3. customobtained
  4. temperatureby cooling in an ice water bath
  5. temperaturethe solution was heated for 30 minutes at 40° C.
  6. stirringNext, while stirring this synthesis solution
  7. customholding at 25° C.
  8. customa solution obtained
  9. temperaturethe solution was heated to 40° C.
  10. temperaturethe clouding increased with time
  11. waitAfter another 20 minutes
  12. additionwere further added
  13. stirringthe solution was stirred for another hour at 40° C.
  14. temperaturecooled
  15. customthe reaction
  16. customNext, crystals obtained
  17. filtrationby filtering this slurry solution
  18. additionwere added to 200 ml of methanol
  19. stirringstirred
  20. washwashed
  21. addition200 ml of methanol were once again added to the crystals
  22. stirringstirred
  23. washwashed
  24. filtrationfiltered
  25. customThe resulting crystals were dried under reduced pressure at 50° C.

출처 및 근거

ORD 기록
ord-2cf66b25d21d4c67abab6115ac9eb043
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790290B2

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