Methanol → HCID 21094286, compound

HRID 1350075Notes

Reaction equation

HRID 1350075 reaction equation
[CH:1]([NH:3][CH2:4][CH:5]([C:10]1[CH:15]=[CH:14][CH:13]=[C:12]([O:16][CH3:17])[CH:11]=1)[C:6]([O:8][CH3:9])=[O:7])=O.P(Cl)(Cl)([Cl:20])=O.CO>C(#N)C>[ClH:20].[CH3:17][O:16][C:12]1[CH:11]=[C:10]2[C:15](=[CH:14][CH:13]=1)[CH:1]=[N:3][CH2:4][CH:5]2[C:6]([O:8][CH3:9])=[O:7]

Participants

5

Reactant 3

HCID 887MethanolHCID 24813Phosphorus oxychlorideHCID 21094283HCID 21094283, compound

Product 1

HCID 21094286HCID 21094286, compound

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Conditions

Temperature
60 °C

Procedure

The compound obtained in Step C (8.03 g; 0.03 mol) is dissolved in 100 ml of acetonitrile, and then the reaction mixture is heated to approximately 60° C. Phosphorus oxychloride (16 ml; 0.17 mol) is added to the solution, which is then heated at reflux for 6 hours with stirring and subsequently evaporated under reduced pressure. The residue obtained is taken up twice with methanol and evaporated under reduced pressure, and then taken up in a minimum of acetone. The precipitate formed is then suction-filtered off to yield the title product in the form of a white solid.

Workup

  1. temperatureis then heated
  2. temperatureat reflux for 6 hours
  3. customsubsequently evaporated under reduced pressure
  4. customThe residue obtained
  5. customevaporated under reduced pressure
  6. customThe precipitate formed
  7. filtrationis then suction-filtered off

Sources & evidence

ORD record
ord-14379690d01e42d8a8d92c99f150bb9d
Source dataset
uspto-grants-2007_05
Patent number
US07214689B2

Reaction notes

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