Phosphorus oxychloride → HCID 21104349, compound

HRID 1354307Notes

Reaction equation

HRID 1354307 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[NH:9][C:10]2[N:11]([N:15]=[CH:16][N:17]=2)[C:12](=O)[CH:13]=1.P(Cl)(Cl)([Cl:20])=O>>[Cl:20][C:12]1[N:11]2[N:15]=[CH:16][N:17]=[C:10]2[N:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])[CH:13]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychloride2×HCID 178515545HCID 178515545, compound

Product 1

HCID 21104349HCID 21104349, compoundYield 46%

Procedure

5-(2-Fluoro-phenyl)-4H-[1,2,4]triazolo[1,5-a]pyrimidin-7-one (840 mg, 3.64 mmole) was suspended in phosphorous oxychloride (5 ml) and heated to reflux for 45 min. Removed excess phosphorous oxychloride under vacuum, the residue treated with ice, extracted product with chloroform, washed chloroform with 10% sodium bicarbonate, dried over sodium sulfate and removed solvent under vacuum to give 420 mg product (yield 46%).

Workup

  1. temperatureheated
  2. temperatureto reflux for 45 min
  3. extractionextracted product with chloroform
  4. washwashed chloroform with 10% sodium bicarbonate
  5. dry with materialdried over sodium sulfate
  6. customremoved solvent under vacuum

Sources & evidence

ORD record
ord-6800ed63ab9b4be39ed6647f8784fb00
Source dataset
uspto-grants-2007_05
Patent number
US07223766B2

Reaction notes

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