Methylcyclohexane → HCID 178443865, compound

HRID 1951961Notes

Reaction equation

HRID 1951961 reaction equation
[O-2].[Nd+3:2].[O-2].[O-2].[Nd+3].[Nd].[N+]([O-])([O-])=O.[Nd+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[CH2:20]([CH:22]([CH2:37][CH2:38][CH2:39][CH3:40])[CH2:23][O:24][P:25](=[O:36])([OH:35])[O:26][CH2:27][CH:28]([CH2:33][CH3:34])[CH2:29][CH2:30][CH2:31][CH3:32])[CH3:21].CC1CCCCC1>O>[CH2:20]([CH:22]([CH2:37][CH2:38][CH2:39][CH3:40])[CH2:23][O:24][P:25]([O-:36])([O:26][CH2:27][CH:28]([CH2:33][CH3:34])[CH2:29][CH2:30][CH2:31][CH3:32])=[O:35])[CH3:21].[Nd+:2]

Participants

7

Reactant 5

HCID 7962MethylcyclohexaneHCID 9275Bis(2-ethylhexyl) phosphateHCID 23934Neodymium2×HCID 159373Neodymium sesquioxideHCID 10980413Neodymium(3+) hydrate trinitrate

Product 1

HCID 178443865HCID 178443865, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2.88 g of neodymium oxide containing 72.4% by weight of neodymium, 0.53 g of an aqueous solution of neodymium nitrate containing 24.4% by weight of neodymium, 17.39 g of di(2-ethylhexyl)phosphoric acid (DEHPA), and 80 g of methylcyclohexane (MCH) are introduced into a reactor made inert beforehand with argon. The mixture is stirred and brought to 80° C. until complete disappearance of the solid, i.e., in this case, 1 h. The mixture is cooled. Three washes with 20 g of water are successively carried out in order to remove the inorganic residues. Each wash comprises a step of stirring for 30 minutes and then a step of separating by settling out, also for 30 minutes, except for the final separating by settling out, which lasts 12 h. The water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus. A clear solution of neodymium di(2-ethylhexyl)phosphate in MCH is thus obtained.

Workup

  1. custombrought to 80° C. until complete disappearance of the solid, i.e., in this case, 1 h
  2. temperatureThe mixture is cooled
  3. customto remove the inorganic residues
  4. stirringof stirring for 30 minutes
  5. customa step of separating
  6. customexcept for the final separating
  7. waitwhich lasts 12 h
  8. distillationThe water/MCH azeotrope is subsequently distilled with a Dean Stark apparatus

Sources & evidence

ORD record
ord-fe5b5a2ec70d47678dea4be2ff829a1a
Source dataset
uspto-grants-2013_03
Patent number
US08404821B2

Reaction notes

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