HRID472833

反应详情

EQUATION

反应方程式

HRID 472833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of methyl 2-(7-chloro-2-(3-chlorophenyl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-hydroxyacetate (5 g, 13.65 mmol) in CH2Cl2 (20 mL) was added Dess-MartinPeriodinane (6.37 g, 15.02 mmol) and the reaction mixture was stirred at room temp for 1 h. The reaction mixture was diluted with ethyl acetate (100 mL). The organic layer was washed with saturated NaHCO3 solution (100 mL) and dried (Na2SO4). The solvent was evaporated and the residue was purified by a quick silica gel chromatography to afford (3.8 g, 76%) of the title compound. 1H NMR (500 MHz, CHLOROFORM-d) δ 8.10-7.98 (m, 1H), 7.89 (td, J=4.4, 1.5 Hz, 1H), 7.51-7.36 (m, 2H), 7.00 (s, 1H), 4.00 (s, 3H), 2.62 (s, 3H).

WORKUP

后处理

  1. washThe organic layer was washed with saturated NaHCO3 solution (100 mL)
  2. dry with materialdried (Na2SO4)
  3. customThe solvent was evaporated
  4. customthe residue was purified by a quick silica gel chromatography