Phosphorus oxide (P4O10) → HCID 14495798, compound

HRID 2292413Notes

Reaction equation

HRID 2292413 reaction equation
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH:9](O)[CH2:10][CH2:11][CH2:12][CH3:13].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>>[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][CH2:10][CH2:11][CH2:12][CH3:13]

Participants

3

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 53793731HCID 53793731, compound

Product 1

HCID 14495798HCID 14495798, compound

Procedure

A solution of compound from Example 16 (55.5 g, 0.28 mol) in light petrol (100 cm3) was added dropwise to a stirred mixture of phosphorus pentoxide (127 g, 0.9 mol) in light petrol (300 cm3). The mixture was stirred overnight at room temperature (GLC analysis revealed reaction to be complete) and then filtered. 5% Palladium-on-charcoal (7 g) was added to the filtrate and the mixture was stirred under an atmosphere of hydrogen (12 h) at room temperature and pressure (GLC analysis revealed reaction to be complete). The palladium-on-charcoal was filtered off and the solvent was removed in vacuo to give the product as a colourless oil which was purified by distillation under reduced pressure.

Workup

  1. custom(GLC analysis revealed reaction to be complete)
  2. filtrationfiltered
  3. addition5% Palladium-on-charcoal (7 g) was added to the filtrate
  4. stirringthe mixture was stirred under an atmosphere of hydrogen (12 h) at room temperature
  5. custompressure (GLC analysis revealed reaction to be complete)
  6. filtrationThe palladium-on-charcoal was filtered off
  7. customthe solvent was removed in vacuo

Sources & evidence

ORD record
ord-84bbd01abbc24b3781db6950ec19596e
Source dataset
uspto-grants-1997_11
Patent number
US05683623

Reaction notes

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