HRID597863

反应详情

EQUATION

反应方程式

HRID 597863 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

Combine 3-(4-chloro-2-fluorobenzyl)-N-(1-(4-methoxybenzyl)-5-methyl-1H-pyrazol-3-yl)-2-methyl-8-(morpholinomethyl)imidazo[1,2-b]pyridazin-6-amine (0.447 g, 0.76 mmol) and trifluoroacetic acid (10 mL) in a 20 mL microwave reactor tube. Seal with a crimp cap then heat in a microwave reactor at 120° C. for 20 min. Partition between EA and water that is made basic with excess NaOH aqueous. Wash the organic phase three times with NaOH aqueous followed by aqueous saturated sodium chloride. Dry over anhydrous magnesium sulfate. Filter and concentrate in vacuo. Purify on silica gel (EA→10% methanol:EA) to give the title compound (0.246 g, 0.52 mmol) as a pale yellow solid. LCMS (8 min)=470.0, M+1.

WORKUP

后处理

  1. customSeal with a crimp
  2. customcap
  3. customPartition between EA and water that
  4. washWash the organic phase three times with NaOH aqueous
  5. dry with materialDry over anhydrous magnesium sulfate
  6. filtrationFilter
  7. concentrationconcentrate in vacuo
  8. customPurify on silica gel (EA→10% methanol:EA)