HRID510206

反应详情

EQUATION

反应方程式

HRID 510206 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of N2-{5-[5-(benzylamino)-1-{[2-(trimethylsilyl)ethoxy]methyl}-1H-pyrrolo[2,3-b]pyridin-3-yl]pyridin-3-yl}-N-(2,2,2-trifluoroethyl)valinamide 5-1a (1.03 g, 1.643 mmol) in MeOH (4 mL) purged with nitrogen (3×) was added palladium hydroxide on carbon (0.540 mg, 0.769 μmol) added and mixture hydrogenated 1 atm for 22 h. The reaction was filtered over Celite and the residue was purified by preparative HPLC reverse phase (C-18), eluting with acetonitrile/water (0.1% TFA), to give product 5-1b. The combined product fractions were basified with NaHCO3, dried over MgSO4, filtered and concentrated. MS APCI: [M+H]+ m/z=537.0.

WORKUP

后处理

  1. additionadded
  2. filtrationThe reaction was filtered over Celite
  3. customthe residue was purified by preparative HPLC reverse phase (C-18)
  4. washeluting with acetonitrile/water (0.1% TFA)