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

HRID 50141

Reaction equation

HRID 50141 reaction equation
[Pd:1].[CH2:2]1[CH2:6][O:5][CH:4]([N:7]2[C:13](=[O:14])[NH:12][C:10](=[O:11])[C:9]([F:15])=[CH:8]2)[CH2:3]1>O>[Pd:1].[CH2:2]1[CH2:6][O:5][CH:4]([N:7]2[C:13](=[O:14])[NH:12][C:10](=[O:11])[C:9]([F:15])=[CH:8]2)[CH2:3]1

Participants

4

Reactant 2

HCID 5386TegafurHCID 23938Palladium

Product 1

HCID 1317224045-Fluoro-1-(oxolan-2-yl)pyrimidine-2,4-dione;palladium

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

Pd was supported on TS-1 by suspending TS-1 (1.6% Ti, 20 grams) in deionized water (80 grams), in the presence of tetraamine palladium nitrate (5% Pd, 2.542 grams) at 80° C. for 24 hours. The solid was recovered by filtration under pressurized N2, washed with deionized water (150 mL, three times), dried under house vacuum at 50° C. overnight, and calcined at 150° C. for 4 hrs in 5% O2-95% N2 mixture. The resulting catalyst has 0.47 wt % Pd. Pd/TS-1 catalyst (2 grams) was then suspended in 75 wt % MeOH -25 wt % H2O (100 grams) and preactivated in a 100 cc/min gas flow (10% C3H6, 4% O2, and 4% H2) at 45 C. and 3 psig for 22 hours.

Workup

  1. filtrationThe solid was recovered by filtration under pressurized N2
  2. washwashed with deionized water (150 mL, three times)
  3. customdried under house vacuum at 50° C. overnight
  4. waitand 3 psig for 22 hours

Sources & evidence

ORD record
ord-93563ea9348a4d5aab947818821a157d
Source dataset
uspto-grants-2004_03
Patent number
US06710192B2

Linked notes

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