Water → 5-Fluoro-1-(oxolan-2-yl)pyrimidine-2,4-dione;palladium

HRID 636846

Reaction equation

[Pd:1](Br)Br.O.[CH2:5]1[CH2:9][O:8][CH:7]([N:10]2[C:16](=[O:17])[NH:15][C:13](=[O:14])[C:12]([F:18])=[CH:11]2)[CH2:6]1>[OH-].[NH4+]>[Pd:1].[CH2:5]1[CH2:9][O:8][CH:7]([N:10]2[C:16](=[O:17])[NH:15][C:13](=[O:14])[C:12]([F:18])=[CH:11]2)[CH2:6]1

Participants

Conditions

Temperature: 23 °C

Procedure

Palladium dibromide (0.377 g) is dissolved in 30% aqueous ammonium hydroxide (50 g) in a 250-mL flask equipped with a magnetic stir bar. Deionized water (60 g) is added to the solution, followed by addition of TS-1 (30 g, 2.12 wt. % titanium) over a 5 minute period. The slurry is stirred at 23° C. for 0.5 hr, then the solvent is removed by rotoevaporation at 55° C. The solids are dried in a vacuum oven (1 torr) at 50° C. for 4 hrs. The catalyst (Catalyst 3) analyzed for 0.5 wt % palladium, 2.1 wt % titanium, 0.7 wt % bromine and 0.37 wt % nitrogen.

Workup

customequipped with a magnetic stir bar
customthe solvent is removed by rotoevaporation at 55° C
customThe solids are dried in a vacuum oven (1 torr) at 50° C. for 4 hrs

Sources & evidence

ORD record: ord-b3db126bc3874a5ea85930bc65e93aff
Source dataset: uspto-grants-2001_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06194591B1

Linked notes

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