HRID2207421

反应详情

EQUATION

反应方程式

HRID 2207421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

Pd/C (10.0 mg, 9.40 mol) was added to a solution of ethyl-3-[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)pyridin-2-yl]prop-2-enoate (96.0 mg, 0.224 mmol) in MeOH (2.00 mL) and THF (1.00 mL). One drop of TFA was added to the reaction mixture and was purged and flushed with argon (3×). The reaction mixture was stirred for 4 hours at room temperature under an atmosphere of hydrogen. The mixture was filtered through CELITE and concentrated under reduced pressure. The residue was purified by silica gel chromatography (3:7 ethyl acetate in hexanes) to afford ethyl 3-[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)pyridin-2-yl]propanoate. C22H22F3N4O2 [M+H]431. found 431.

WORKUP

后处理

  1. customwas purged
  2. customflushed with argon (3×)
  3. filtrationThe mixture was filtered through CELITE
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by silica gel chromatography (3:7 ethyl acetate in hexanes)