Phosphorus oxychloride → HCID 15679424, compound

HRID 257410Notes

Reaction equation

HRID 257410 reaction equation
[C:1]([N:5]1[C:14](=[O:15])[C:13]2[CH:12]=[C:11]([CH3:16])[N+:10]([O-])=[CH:9][C:8]=2[C:6]1=[O:7])([CH3:4])([CH3:3])[CH3:2].P(Cl)(Cl)([Cl:20])=O>>[C:1]([N:5]1[C:14](=[O:15])[C:13]2[CH:12]=[C:11]([CH2:16][Cl:20])[N:10]=[CH:9][C:8]=2[C:6]1=[O:7])([CH3:4])([CH3:3])[CH3:2]

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 15679423HCID 15679423, compound

Product 1

HCID 15679424HCID 15679424, compound

Procedure

31.5 g of N-tert-butyl-6-methylpyridine-3,4-dicarboximide-1-oxide from 6.004 are added a little at a time to 300 ml of phosphorus oxychloride, and the mixture is heated stepwise until it refluxes and is stirred for 3 hours. The reaction mixture is evaporated down under reduced pressure, the residue is taken up in methylene chloride and the solution is stirred into ice water. The organic phase is washed several times with water, dried, filtered over alumina and evaporated down under reduced pressure. 28.9 g of the title compound of melting point 62°-64° C. are obtained.

Workup

  1. temperaturethe mixture is heated stepwise until it
  2. customThe reaction mixture is evaporated down under reduced pressure
  3. stirringthe solution is stirred into ice water
  4. washThe organic phase is washed several times with water
  5. customdried
  6. filtrationfiltered over alumina
  7. customevaporated down under reduced pressure

Sources & evidence

ORD record
ord-323b9cc36da944dbb7bed86ded2cf796
Source dataset
uspto-grants-1993_11
Patent number
US05262384

Reaction notes

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