HRID2097398

反应详情

EQUATION

反应方程式

HRID 2097398 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Reaction was carried out in the same manner as in Example 1-(b) except for using 51 mg (0.090 mmol) of 2-(3-cyclopropoxy-4-difluoromethoxyphenyl)-3-hydroxyphenylmethyl-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo-[2,3-d]pyridazin-4-one obtained in Example 20-(a) in place of 2-(3-cyclopropoxy-4-difluoromethoxyphenyl)-1-(2-trimethylsilylethoxymethyl)-1,5-dihydropyrrolo[2,3-d]pyridazin-4-one. After completion of the reaction, water was added to the reaction mixture, and the mixture was extracted with a mixed solvent (chloroform:methanol=9:1 (V/V)). The organic layer after separating the liquids was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The obtained residue was applied to silica gel column chromatography (Eluent; hexane:ethyl acetate=9:1 (V/V)), and the fractions containing the desired compound were concentrated under reduced pressure to obtain 17 mg of the title compound as a white solid. (Yield: 42%)

WORKUP

后处理

  1. customReaction
  2. additionwas added to the reaction mixture
  3. extractionthe mixture was extracted with a mixed solvent (chloroform:methanol=9:1 (V/V))
  4. customThe organic layer after separating the liquids
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure
  7. additionthe fractions containing the desired compound
  8. concentrationwere concentrated under reduced pressure