Reaction #1797488

ord-f3aaec8856f24ac2b20a52a986e169b1

Reaction equation

O=[N+]([O-])[O-].O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Nd+3]
neodymium nitrate
O=[N+]([O-])[O-].O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Nd+3]
neodymium nitrate
CCN(CC)CC
triethylamine
O=[N+]([O-])[O-].O=[N+]([O-])[O-].O=[N+]([O-])[O-].[Nd+3]
neodymium nitrate
O=C(O)COc1ccccc1
phenoxyacetic acid
O=C(O)COc1ccccc1
phenoxyacetic acid
[Nd]
neodymium

Conditions

Temperature
25°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherSpecifically, a reactor similar to that of 1-1 was used
  2. 2
    workup.STIRRINGto stir a solution
  3. 3
    Otherobtained
  4. 4
    Temperatureby cooling in an ice water bath
  5. 5
    Temperaturethe solution was heated for 30 minutes at 40° C.
  6. 6
    TemperatureNext, this synthesis solution was maintained at about 30° C.
  7. 7
    Othera solution obtained
  8. 8
    workup.STIRRINGwhile stirring
  9. 9
    Temperaturethe clouding increased with time
  10. 10
    Other30 minutes
  11. 11
    Temperaturethe solution was heated to 40° C. for 30 minutes

Procedure

The compound was synthesized by the same method as that for Synthesis Example 1-2 above, that is, after forming a triethylamine salt of phenoxyacetic acid in anhydrous methanol, a methanol solution of neodymium nitrate was added while stirring. Specifically, a reactor similar to that of 1-1 was used to stir a solution obtained by adding 100 ml of an anhydrous methanol to 45.65 g (0.3 mol) of phenoxyacetic acid, while dripping 30.4 g (0.3 mol) of triethylamine while maintaining at 25° C. by cooling in an ice water bath. After dripping, the solution was heated for 30 minutes at 40° C. to prepare a transparent synthesis solution of phenoxyacetic acid-triethylamine salts. Next, this synthesis solution was maintained at about 30° C., and a solution obtained by dissolving 43.8 g of neodymium nitrate into 100 ml of methanol was dripped in while stirring. Upon completion of the dripping of the neodymium nitrate solution, it began to cloud, and the clouding increased with time. 30 minutes after completion of dripping, the solution was heated to 40° C. for 30 minutes, to produce a slurry solution of a neodymium salt of phenoxyacetic acid. 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 38.8 g of a neodymium salt of phenoxyacetic acid (yield 65%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07790290B2uspto-grants-2010_09