HRID1989891

反应详情

EQUATION

反应方程式

HRID 1989891 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of 3-[(1S)-2-methoxy-(1-methylethyl)oxy]-N-(1-methyl-1H-pyrazol-3-yl)-5-[(phenylmethyl)oxy]benzamide (7.07 g) in THF (50 mL) and methanol (50 mL) was added 10% palladium on carbon (727 mg) as a slurry in THF (1 mL) and methanol (1 mL). The mixture was placed under vacuum and stirred under an atmosphere of hydrogen for 70 hours. The mixture was filtered through diatomaceous earth, and the diatomaceous earth washed with methanol (2×100 mL), followed by evaporation in vacuo. The residues were dissolved in ethyl acetate (10 mL), treated with isohexane (40 mL), the solid filtered off and washed with isohexane (50 mL) to afford the desired compound (5.17 g) which was used without further purification.

WORKUP

后处理

  1. filtrationThe mixture was filtered through diatomaceous earth
  2. washthe diatomaceous earth washed with methanol (2×100 mL)
  3. customfollowed by evaporation in vacuo
  4. dissolutionThe residues were dissolved in ethyl acetate (10 mL)
  5. additiontreated with isohexane (40 mL)
  6. filtrationthe solid filtered off
  7. washwashed with isohexane (50 mL)