From 5 - fluorouracil by chlorination, ammoniation, hydrolysis obtained 0.1. Chlorination 5-Fluorouracil and phosphorus oxychloride were added to the chlorination pot, stirred, controlled at 20 below the dropwise addition of N, N-dimethylaniline. After the addition was completed, the reaction was heated to about 110 C for 2 hours. Cool to room temperature, put it in ice and brine, and keep stirring at 15 for 1 hour. Filtered and washed with water to give 2,4-dichloro-5-fluoropyrimidine 0.2. Ammonia 2,4-Dichloro-5-fluoropyrimidine dissolved in ethanol, stirring, controlled at 35 below ammonia solution. Bi completed, cooled to 25 C for 3 hours, vacuum recovery of ethanol to dryness, heated to 20 with stirring. Filtration, washing of the crystals with water and drying gave 4-amino-2-chloro-5-fluoropyrimidine 0.3. Hydrolysis 4-amino-2-chloro-5-fluoropyrimidine and hydrochloric acid were mixed, heated to 90-95 C with stirring, the reaction 2 hours, concentrated under reduced pressure to dryness, dissolved in water and crystallization, activated carbon decolorization. Filtration, the filtrate was adjusted to pH 7-8 with ammonia, placed overnight rejection filter, washed with water crystallization, the purified fluoridagenimid. The total yield of 50%. The starting material of the method for the anticancer drug fluorouracil [51-21-8], can also be used fluorouracil precursor, that is, 2-methoxy-4-hydroxy-5-fluoropyrimidine as raw material, the chloride, ammonia Preparation of flucytosine, hydrolysis, yield 70%. The above precursor was added to toluene, and then added dimethylaniline, heated to 50-60 C, phosphorus oxychloride dropwise. Then 105-110 C for 3 hours. After cooling to room temperature, the reaction mixture was added to a mixture of toluene and water and stirred at 25-40 C. The toluene layer was separated and the aqueous layer was extracted with toluene. The liquid and the toluene layer were combined and the toluene was recovered under reduced pressure. The distillate of 86-90 C. (2.66 kPa) was collected to obtain 2-methoxy-4-chloro- 5-fluoropyrimidine. The above step chlorinated product and anhydrous methanol was added to the autoclave at room temperature through ammonia to saturation, slowly warming so that the pressure reaches 0.5MPa, the reaction was stirred overnight. Cold to room temperature, the material was treated to give 2-methoxy-4-amino-5-fluoropyrimidine, mp 189-191 C. This was reacted with 30% hydrochloric acid at 100-105 C for 3 hours. Hydrolyzate is evaporated to dryness under reduced pressure, the residue is dissolved in water, alkalinized with ammonia to pH8.5, cooled to below 5 C, filtered to give crude flucytosine, recrystallized from water to obtain the finished product.
Usage of Fluorocytosine
1. used to make antidiabetic
2. a toxic antifungal/antimicrobial agent
1. Advanced Technology with good quality
2. Usually have 1MT on stock
Xinxiang Aurora Biotechnology Co., Ltd.
No. 348, Pingyuan Road, Xinxiang City, Henan Province, China 453000
DUNS Number: 544 530 473
Phone: 186 373 52520
Contact: Felix Cao