HRID221996

反应详情

EQUATION

反应方程式

HRID 221996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A mixture of 2,2,2-trifluoro-N-(3-methyl-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutyl)acetamide (4-12) (3.3 mg, 0.006 mmol) and NaOH (5M in water, 0.30 mL) in EtOH (3 mL) was stirred at 70° C. for 15 hours. The mixture was diluted with CHCl3, washed with water and 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 3-methyl-1-{-4-[9-phenyl-3-(2-pyrimidinyl)[1,2,4]triazolo[3,4-f]-1,6-naphthyridin-8-yl]phenyl}cyclobutanamine (4-13) as a white form. HRMS (M+H)+: observed=484.2250, calculated=484.2243.

WORKUP

后处理

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