Tegafur synthesis
- Product Name:Tegafur
- CAS Number:17902-23-7
- Molecular formula:C8H9FN2O3
- Molecular Weight:200.17
Yield:17902-23-7 92.35%
Reaction Conditions:
with dihydrogen peroxide;copper diacetate in N,N-dimethyl-formamide at 40; for 5 h;Reagent/catalyst;Time;Solvent;Temperature;
Steps:
1-13 Example 1
5-Fluorouracil (13.00 g, 0.10 mol), tetrahydrofuran (11.54 g, 0.16 mol), copper acetate (399.30 mg, 2.0 mmol), hydrogen peroxide solution (28.33 g, 0.25 mol, 30%),N, N-dimethylformamide (150mL) was added to the flask, stirred, heated to 40 ° C, reacted for 5h, filtered, and the filtrate was poured into a mixed solution of ice water (500mL) and ethyl acetate (300mL). After stirring for 15 min, the layers were separated. The organic phase was washed with purified water (100 mL × 3) and saturated brine (100 mL) in that order, dried over anhydrous sodium sulfate, and the filtrate was concentrated under reduced pressure to dryness to obtain the crude tegafur. After recrystallization, a tegafur refined product was obtained with a yield of 92.35%. According to HPLC detection, tR = 13.926min was tegafur with a purity of 99.952% and a maximum single impurity of 0.016%.
References:
Lunan Pharmaceutical Group Co., Ltd.;Zhang Guimin;Bao Guanglong;Zhang Xianli CN110655506, 2020, A Location in patent:Paragraph 0035-0056
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