Phosphorus oxychloride → HCID 53408117, compound

Reaction equation

Br.[Br:2][C:3]1[CH:4]=[N:5][C:6](=O)[NH:7][CH:8]=1.P(Cl)(Cl)([Cl:12])=O>>[ClH:12].[Br:2][C:3]1[C:4]([Cl:12])=[N:5][CH:6]=[N:7][CH:8]=1

Participants

Reactant 2

HCID 24813Phosphorus oxychloride

HCID 127955335-Bromopyrimidin-2(1H)-one hydrobromide

Product 1

HCID 53408117HCID 53408117, compound

Conditions

Temperature: 90 °C

Procedure

A suspension of 5-bromopyrimidone hydrobromide (1.0 g, 3.9 mmol) in phosphorous oxychloride (4 mL) was heated at 90° C. for 1 h then cooled 0° C. The mixture was filtered, washed with POCl3 (2×2 mL) to furnish the title compound as a cream solid (388 mg). This compound was unstable to air and was used immediately in the next step.

Workup

temperaturethen cooled 0° C
filtrationThe mixture was filtered
washwashed with POCl3 (2×2 mL)

Sources & evidence

ORD record: ord-688f370ec4aa487a9a170614f2ba51b7
Source dataset: uspto-grants-2014_07
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08778925B2

Reaction notes

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