HRID6886

反应详情

EQUATION

反应方程式

HRID 6886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 5-{[2-(6-bromo-pyridin-2-ylamino)-thiazol-5-ylmethyl]-amino}-N-cyclopropyl-2,4-difluoro-benzamide (96 mg, 0.20 mmol) in neat N-methyl piperazine (0.4 mL) was heated to 120° C. in a sealed tube for 5 h. The reaction mixture was cooled to RT, diluted with methylene chloride (5 mL), and washed with water (2×5 mL). The organic layer was dried over Na2SO4, concentrated, and the residue was purified by silica gel eluted with 2-10% MeOH/CH3Cl to give the title compound (53 mg, 55%) as a light yellow solid. (M+H)+=500.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to RT
  2. washwashed with water (2×5 mL)
  3. dry with materialThe organic layer was dried over Na2SO4
  4. concentrationconcentrated
  5. customthe residue was purified by silica gel
  6. washeluted with 2-10% MeOH/CH3Cl