HRID1358066

反应详情

EQUATION

反应方程式

HRID 1358066 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThe solution thus obtained
  2. concentrationis concentrated under vacuum
  3. concentrationis concentrated to a small volume and, after 15 hours at room temperature
  4. filtrationthe precipitate is filtered
  5. washwashed with ethyl acetate
  6. customdried