HRID1358066
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 95 °C
PROCEDURE
实验过程
A suspension of 51 g (0.105 m) of 5′-deoxy-5′-iodo-2′,3′-O-isopropylidene-5-fluorouridine in 500 ml of acetic acid and 120 ml of water is heated at 95° C. for 90 minutes. The solution thus obtained is concentrated under vacuum and the residue is taken up with 2 l of ethyl acetate, then is concentrated to a small volume and, after 15 hours at room temperature, the precipitate is filtered, washed with ethyl acetate and dried to give 35.6 g of 5′-deoxy-5′-iodo-5-fluoro uridine. M.p.=174.5÷175.5° C., purity (HPLC)=99.74% [α]D=+8.96° (c=1.00, CH3OH).
WORKUP
后处理
- customThe solution thus obtained
- concentrationis concentrated under vacuum
- concentrationis concentrated to a small volume and, after 15 hours at room temperature
- filtrationthe precipitate is filtered
- washwashed with ethyl acetate
- customdried