HRID2063603

反应详情

EQUATION

反应方程式

HRID 2063603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

[2-(6-{N′-[1-(4-dimethylamino-phenyl)-ethylidene]-hydrazino}-2-methyl-pyrimidin-4-yl)-phenyl]-carbamic acid tert-butyl ester was dissolved in 10 mL of 5% trifluoroacetic acid in dichloromethane. The resultant reaction mixture was stirred at room temperature for 2 hours before being concentrated in vacuo. The residue was dissolved in methanol and the pH was adjusted to 7 with potassium bicarbonate. After filtration the methanol was concentrated in vacuo and the residue was purified by Si gel chromatography (1:1 ethyl acetate:hexanes) yielding 140 mg (60%) of the title compound as a brown solid. HPLC Purity: 95%.

WORKUP

后处理

  1. customThe resultant reaction mixture
  2. concentrationbefore being concentrated in vacuo
  3. dissolutionThe residue was dissolved in methanol
  4. filtrationAfter filtration the methanol
  5. concentrationwas concentrated in vacuo
  6. customthe residue was purified by Si gel chromatography (1:1 ethyl acetate:hexanes)