HRID221993

反应详情

EQUATION

反应方程式

HRID 221993 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2,2,2-trifluoro-N-(3-oxo-1-{4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-2) (25 mg, 0.043 mmol), trimethylsilyl cyanide (0.012 mL, 0.086 mmol), and zinc iodide (1.4 mg, 0.0043 mmol) in CH2Cl2 (1.0 mL) was stirred at room temperature for 1 hour. To the mixture was added water, extracted with CHCl3, washed with brine, dried (MgSO4), filtered, and the solvent was removed under reduced pressure. The residue was purified by preparative TLC, eluting with 10% MeOH in CHCl3 to give N-(3-cyano-3-hydroxy-1-{4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)-2,2,2-trifluoroacetamide (4-10) as a yellow solid. MS (M+H)+: observed=607, calculated=607.

WORKUP

后处理

  1. extractionextracted with CHCl3
  2. washwashed with brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by preparative TLC
  7. washeluting with 10% MeOH in CHCl3