Phosphorus oxychloride → HCID 53407931, compound

HRID 1622332

Reaction equation

[CH3:1][C:2]1[C:3](=O)[NH:4][CH:5]=[N:6][CH:7]=1.P(Cl)(Cl)([Cl:11])=O>>[ClH:11].[Cl:11][C:3]1[C:2]([CH3:1])=[CH:7][N:6]=[CH:5][N:4]=1

Participants

Reactant 2

HCID 24813Phosphorus oxychloride

HCID 2053244-Pyrimidinol, 5-methyl-

Product 1

HCID 53407931HCID 53407931, compound

Conditions

Temperature: 90 °C

Procedure

A mixture of 5-methyl-3H-pyrimidin-4-one (0.60 g, 3.6 mmol) and phosphorous oxychloride (2.0 mL) was heated at 90° C. for 2.5 h. The mixture was evaporated to dryness under reduced pressure and the resultant solid was purified by sublimation under reduced pressure to furnish the title compound as a white solid. This compound was unstable to air and was used immediately in the next step.

Workup

customThe mixture was evaporated to dryness under reduced pressure
customthe resultant solid was purified by sublimation under reduced pressure

Sources & evidence

ORD record: ord-5c6992e2e2cc4d99b61018019e5c64be
Source dataset: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08778925B2

Linked notes

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