HRID1802464

反应详情

EQUATION

反应方程式

HRID 1802464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of 5-amino-2,4-dimethyl-N-(pyridin-3-ylmethyl)benzenesulfonamide (300 mg, 1.0 mmol) and 1,5-dichloro-9-fluorobenzo[c]-2,6-naphthyridine (Example 1, Step 5) (250 mg, 0.94 mmol) in THF (4.7 mL) at 0° C. was added NaHMDS (2.8 mL, 1 M in THF, 2.8 mmol). The deep red solution was stirred at 0° C. for ten minutes and then quenched by the addition of sat. aq. NaHCO3 solution. The reaction was extracted with EtOAc and the organic extracts were dried over Na2SO4 and concentrated in vacuo. Purification by silica gel column chromatography (0-5% MeOH/DCM) afforded the title compound.

WORKUP

后处理

  1. customquenched by the addition of sat. aq. NaHCO3 solution
  2. extractionThe reaction was extracted with EtOAc
  3. dry with materialthe organic extracts were dried over Na2SO4
  4. concentrationconcentrated in vacuo
  5. customPurification by silica gel column chromatography (0-5% MeOH/DCM)