Acetone → O-[2-(2,6-dimethyl-3-pyridylamino)-2-ketoethyl] O-methyl O-(4-chlorophenyl) phosphate

HRID 1973233

Reaktionsgleichung

Reaktionsgleichung von HRID 1973233
[CH3:1][C:2]1[C:7]([NH:8][C:9](=[O:12])[CH2:10]Cl)=[CH:6][CH:5]=[C:4]([CH3:13])[N:3]=1.[P:14]([O-:26])([O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)([O:16][CH3:17])=[O:15].[K+].CC(C)=O>CCOCC>[P:14]([O:18][C:19]1[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=1)([O:16][CH3:17])([O:26][CH2:10][C:9]([NH:8][C:7]1[C:2]([CH3:1])=[N:3][C:4]([CH3:13])=[CH:5][CH:6]=1)=[O:12])=[O:15]

Komponenten

5

Edukt 3

HCID 180AcetoneHCID 21493317N-(2,6-dimethyl-3-pyridyl)-alpha-chloroacetamideHCID 68134157potassium O-methyl O-(4-chlorophenyl) phosphate

Produkt 1

HCID 54372328O-[2-(2,6-dimethyl-3-pyridylamino)-2-ketoethyl] O-methyl O-(4-chlorophenyl) phosphate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

N-(2,6-Dimethyl-3-pyridyl)-α-chloroacetamide (32.2 grams), potassium O-methyl O-(4-chlorophenyl) phosphate (26 grams) and acetone (200 ml) are charged into a glass reaction vessel equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is heated at reflux for a period of about 24 hours. After this time the mixture is stripped of solvent on a steam bath and the resulting residue is dissolved in ether. The ether solution is washed with water and is dried over magnesium sulfate. The dried solution is then evaporated under vacuum to yield the desired product O-[2-(2,6-dimethyl-3-pyridylamino)-2-ketoethyl] O-methyl O-(4-chlorophenyl) phosphate.

Aufarbeitung

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. temperatureThe reaction mixture is heated
  4. temperatureat reflux for a period of about 24 hours
  5. customAfter this time the mixture is stripped of solvent on a steam bath
  6. washThe ether solution is washed with water
  7. dry with materialis dried over magnesium sulfate
  8. customThe dried solution is then evaporated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-9a4d6d8b58a642e29525e9cf6126711e
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03996352

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