HRID2279128

反应详情

EQUATION

反应方程式

HRID 2279128 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

To a solution of 150 mg of methanesulfonic acid 6-(4-methoxymethoxy-phenyl)-3-methyl-1-(tetrahydro-pyran-2-yl)-1H-pyrazolo[3,4-b]pyridin-4-ylmethyl ester, and 85 mg 2,5,5-trimethyl-1-(pyridin-3-ylmethyl)piperazine in 4 ml of dry THF were added 0.28 ml of DIPEA. The reaction was heated to 140° C. for 60 min in a microwave reactor. The reaction was diluted with ethyl acetate and water and the aqueous phase was extracted with ethyl acetate. The combined organic phases were dried over sodium sulphaste, filtrated and concentrated. The resulting oil was purified by chromatography (silica, heptanes/ethyl acetate). 69 mg of the title compound were obtained.

WORKUP

后处理

  1. extractionthe aqueous phase was extracted with ethyl acetate
  2. dry with materialThe combined organic phases were dried over sodium sulphaste
  3. filtrationfiltrated
  4. concentrationconcentrated
  5. customThe resulting oil was purified by chromatography (silica, heptanes/ethyl acetate)