Phosphorus oxychloride → HCID 15672756, compound

HRID 704497Notes

Reaction equation

HRID 704497 reaction equation
P(Cl)(Cl)([Cl:3])=O.O[C:7]1[N:12]2[N:13]=[C:14]([CH2:16][O:17][CH3:18])[N:15]=[C:11]2[N:10]=[C:9]([CH3:19])[CH:8]=1>CN(C)C1C=CC=CC=1>[Cl:3][C:7]1[N:12]2[N:13]=[C:14]([CH2:16][O:17][CH3:18])[N:15]=[C:11]2[N:10]=[C:9]([CH3:19])[CH:8]=1

Participants

4

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178494657HCID 178494657, compound

Product 1

HCID 15672756HCID 15672756, compound

Reagents, catalysts & solvents 1

HCID 949N,N-DimethylanilineSolvent

Procedure

To a mixed solution of 300 ml of phosphorus oxychloride and 50 ml of N,N-dimethylaniline was added 38.8 g of 7-hydroxy-2-methoxymethyl-5-methyl-s-triazolo[1,5-a]pyrimidine, and the mixture was stirred at 50° to 60° C. for one hour. After removing phosphorus oxychloride, the residue was dissolved in 500 ml of chloroform and stirred by adding ice. The chloroform layer was separated and washed with water, and then dried over anhydrous magnesium sulfate and distilled the solvent to obtain crystals. The crystals were collected by filtration and washed with water, and then dried to obtain the title compound.

Workup

  1. customAfter removing phosphorus oxychloride
  2. dissolutionthe residue was dissolved in 500 ml of chloroform
  3. stirringstirred
  4. additionby adding ice
  5. customThe chloroform layer was separated
  6. washwashed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationdistilled the solvent
  9. customto obtain crystals
  10. filtrationThe crystals were collected by filtration
  11. washwashed with water
  12. customdried

Sources & evidence

ORD record
ord-c3a0cc83a23f40deb9b07bbc688f1cc5
Source dataset
uspto-grants-1991_01
Patent number
US04987129

Reaction notes

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