HRID2255921

反应详情

EQUATION

反应方程式

HRID 2255921 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washwashed with aqueous sodium carbonate solution
  2. dry with materialdried (MgSO4)
  3. customthe solvent evaporated
  4. customThe residual solid was purified by flash chromatography (Merck 9385)