Phosphorus oxide (P4O10) → 84141-80-0

HRID 434523Notes

Reaction equation

HRID 434523 reaction equation
[CH3:1][C:2]1([C:12]([NH2:14])=O)[O:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4][CH2:3]1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C1(C)C=CC=CC=1>[C:12]([C:2]1([CH3:1])[O:7][C:6]2[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=2[O:4][CH2:3]1)#[N:14]

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 13035181HCID 13035181, compound

Product 1

HCID 1303518284141-80-0Yield 69.9%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

A stirred mixture of 2-methyl-1,4-benzodioxan-2-carboxamide (8.17 g), phosphorus pentoxide (17 g) and anhydrous toluene (175 ml) was heated under reflux for 4 hours. On cooling the supernatant was decanted from the residue, the latter being washed by decantation with more toluene. Filtration and evaporation of the solvent gave a solid residue (5.18 g). Crystallisation from ethanol yielded the cyano compound (4.4 g); m.p. 88°-89°.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hours
  3. temperatureOn cooling the supernatant
  4. customwas decanted from the residue
  5. washthe latter being washed by decantation with more toluene
  6. filtrationFiltration and evaporation of the solvent

Sources & evidence

ORD record
ord-d2293c3eeb2f4f1a884dea80100370e0
Source dataset
uspto-grants-1983_08
Patent number
US04397860

Reaction notes

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