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

HRID 50141

반응식

HRID 50141 반응식
[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

참가 물질

4

반응물 2

HCID 5386TegafurHCID 23938Palladium

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-93563ea9348a4d5aab947818821a157d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710192B2

연결된 노트

불러오는 중…