HRID2255921
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
PROCEDURE
实验过程
Trifluoromethanesulphonic anhydride (0.85 ml, 5 mM) was added dropwise to a stirred solution of 1,6-dimethyl-4-hydroxypyridin-2-one [0.7 g, 5 mM] (obtainable as described by Castillo et al., Bull. Soc. Chim. France, 1982, 257) in dry methylene chloride (15 ml). The resulting solution was kept at room temperature for 18 hours, washed with aqueous sodium carbonate solution, dried (MgSO4) and the solvent evaporated. The residual solid was purified by flash chromatography (Merck 9385) using ether as eluant to give 1,6-dimethyl-4-(trifluoromethanesulphonyloxy)-2-pyridone as a solid (0.67 g), m.p. 65°-67° C.; NMR: 2.41(3H,s, CH3) 3.53(3H,s, NCH3), 6.05(1H,s, CH), 6.38(1H,s, CH).
WORKUP
后处理
- washwashed with aqueous sodium carbonate solution
- dry with materialdried (MgSO4)
- customthe solvent evaporated
- customThe residual solid was purified by flash chromatography (Merck 9385)