HRID1953965
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
- 165 °C
PROCEDURE
实验过程
A solution of 3-benzyloxy-5-(methylsulfonyl)-2-thiopenecarboxylic acid (13.6 g, 43.6 mmol) in 50 ml quinoline is treated with Cu powder (4.15 g, 65.4 mmol) at room temperature, heated to 165° C. for 15 minutes, cooled to room temperature and filtered. (The filtercake is washed with water.) The combined filtrate is acidified to pH 1 with 6N HCl and filtered. This filtercake is washed with water and dried to afford the title product as a dark grey powder, 10.1 g (86% yield), mp 108-109° C., identified by 1HNMR, 13CNMR and mass spectral analyses.
WORKUP
后处理
- temperaturecooled to room temperature
- filtrationfiltered
- wash(The filtercake is washed with water
- filtrationfiltered
- washThis filtercake is washed with water
- customdried