Phosphorus oxide (P4O10) → HCID 12260172, compound

HRID 328461Notes

Reaction equation

HRID 328461 reaction equation
[C:1]([CH:3]([NH:5]/[C:6](=[C:9](\[NH2:12])/[C:10]#[N:11])/[C:7]#[N:8])[CH3:4])#N.[O:13]=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>C(O)C>[C:10]([C:9]1[NH:12][C:4](=[O:13])[CH:3]([CH3:1])[NH:5][C:6]=1[C:7]#[N:8])#[N:11]

Participants

4

Reactant 2

HCID 14812Phosphorus oxide (P4O10)HCID 45122244HCID 45122244, compound

Product 1

HCID 12260172HCID 12260172, compoundYield 420.2%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 1.0 g of α-cyanoethyldiaminomaleonitrile obtained as described in Example 4 and 0.3 g of phosphorus pentoxide was heated under refluxing for 19 hours in 30 ml of ethanol. Thereafter, the solvent was distilled off, and the resulting residue was treated with ice-water to obtain brown-colored fine crystals. The crystals thus obtained were recrystallized from a mixture of tetrahydrofuran, methanol and water (2:2:1 by volume) to obtain 0.72 g (72% yield) of 5,6-dicyano-2-methyl-1,2,3,4-tetrahydropyrazin-3-one having a melting point of 243°-245° C as a white powder.

Workup

  1. customobtained
  2. temperaturewas heated
  3. distillationThereafter, the solvent was distilled off
  4. additionthe resulting residue was treated with ice-water
  5. customto obtain brown-colored fine crystals
  6. customThe crystals thus obtained
  7. customwere recrystallized from a mixture of tetrahydrofuran, methanol and water (2:2:1 by volume)

Sources & evidence

ORD record
ord-4d018203176445d19893ac68911d7948
Source dataset
uspto-grants-1977_04
Patent number
US04017533

Reaction notes

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