HRID1274865

反应详情

EQUATION

反应方程式

HRID 1274865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Lithium bis(trimethylsilyl)amide (1.5 ml of 1.0M solution) was added to a solution of 1-(3,5-difluorophenyl)-2-(2,3-dihydro-6-methyl-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropan-1-one (0.5 g) in tetrahydrofuran, under inert atmosphere at -5° C. After stirring for 0.5 hours, the solution was poured onto solid carbon dioxide (excess), allowed to warm to ambient temperature and poured onto water. The aqueous phase was acidified, extracted (ethyl acetate), dried (magnesium sulphate) and evaporated, to give 1-(3,5-difluorophenyl)-2-(6-carboxymethyl-2,3-dihydro-4-oxo-5-phenyl-4H-1,3-oxazin-3-yl)-2-methylpropan-1-one (Compound 704, 0.065 g), NMR 1.5 (s,6H), 3.2 (s,2H), 5.4 (s,2H), 6.8 (m,1H), 7.0 (m,2H), 7.2 (m,3H), 7.5 (d,2H), 9.0 (bs,1H).

WORKUP

后处理

  1. additionpoured onto water
  2. extractionextracted (ethyl acetate)
  3. dry with materialdried (magnesium sulphate)
  4. customevaporated