Phosphorus oxychloride → HCID 86685394, compound

HRID 570736Notes

Reaction equation

HRID 570736 reaction equation
C([O:3][C:4]1[N:5]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]([F:27])([F:26])[F:25])=[CH:18][CH:17]=2)[C:6](=[O:15])[C:7]2[CH:13]=[CH:12][NH:11][C:10](=O)[C:8]=2[N:9]=1)C.P(Cl)(Cl)([Cl:30])=O>>[Cl:30][C:10]1[C:8]2[NH:9][C:4](=[O:3])[N:5]([C:16]3[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]([F:27])([F:26])[F:25])=[CH:18][CH:17]=3)[C:6](=[O:15])[C:7]=2[CH:13]=[CH:12][N:11]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 68015337HCID 68015337, compound

Product 1

HCID 86685394HCID 86685394, compound

Conditions

Temperature
100 °C

Procedure

A mixture of 2-ethoxy-3-[4-(2,2,2-trifluoroethoxy)phenyl]-3,7-dihydropyrido[3,4-d]pyrimidine-4,8-dione (763 mg) and phosphorus oxychloride (10 ml) was stirred at 100° C. for 5 hr, allowed to be cooled to room temperature, and concentrated under reduced pressure. To the residue was added toluene, and the mixture was again concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound (437 mg).

Workup

  1. temperatureto be cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue was added toluene
  4. concentrationthe mixture was again concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)

Sources & evidence

ORD record
ord-cc1cd6a3b8884e94b86cca25ba486861
Source dataset
uspto-grants-2015_05
Patent number
US09023858B2

Reaction notes

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