Methylcyclohexane → HCID 178443865, compound

HRID 1951962Notes

Reaction equation

HRID 1951962 reaction equation
[O-2].[Nd+3:2].[O-2].[O-2].[Nd+3].[Nd].[Cl-].[Nd+3].[Cl-].[Cl-].[CH2:11]([CH:13]([CH2:28][CH2:29][CH2:30][CH3:31])[CH2:14][O:15][P:16](=[O:27])([OH:26])[O:17][CH2:18][CH:19]([CH2:24][CH3:25])[CH2:20][CH2:21][CH2:22][CH3:23])[CH3:12].CC1CCCCC1>O>[CH2:11]([CH:13]([CH2:28][CH2:29][CH2:30][CH3:31])[CH2:14][O:15][P:16]([O-:27])([O:17][CH2:18][CH:19]([CH2:24][CH3:25])[CH2:20][CH2:21][CH2:22][CH3:23])=[O:26])[CH3:12].[Nd+:2]

Participants

7

Reactant 5

HCID 7962MethylcyclohexaneHCID 9275Bis(2-ethylhexyl) phosphateHCID 23934Neodymium2×HCID 1593731313-97-9HCID 10131187Neodymium(3+) trichloride

Product 1

HCID 178443865HCID 178443865, compoundYield 98%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

2.88 g of neodymium oxide containing 72.4% by weight of neodymium, 0.58 g of an aqueous solution of neodymium chloride containing 22.2% 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. for 5 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. temperatureThe mixture is cooled
  2. customto remove the inorganic residues
  3. stirringof stirring for 30 minutes
  4. customa step of separating
  5. waitby settling out, also for 30 minutes
  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-e438d8d9870d46d4ae39a79179635b02
Source dataset
uspto-grants-2013_03
Patent number
US08404821B2

Reaction notes

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