HRID490117

反应详情

EQUATION

反应方程式

HRID 490117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

6-methyl-3-(6-(methylsulfinyl)pyrimidin-4-yl)pyrazolo[1,5-a]pyrimidin-2-amine (60 mg, 0.21 mmol) was dissolved in NMP with nipecotamide (100 mg, 0.78 mmol)and heated to 200° C. in a microwave for 20 min. The reaction mixture was purified by RP HPLC (C18, CH3CN/H2O 0.1% TFA) and the pure fractions were poured into ethyl acetate/0.5 N NaOH. The organic phase was dried over sodium sulfate and concentrated to a yellow solid which was dissolved in 1N HCl in MeOH and concentrated to the HCl salt as a yellow solid, 20 mg, 0.052 mmol, 26%. LC/MS MH+353.4

WORKUP

后处理

  1. customThe reaction mixture was purified by RP HPLC (C18, CH3CN/H2O 0.1% TFA)
  2. additionthe pure fractions were poured into ethyl acetate/0.5 N NaOH
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. concentrationconcentrated to a yellow solid which
  5. dissolutionwas dissolved in 1N HCl in MeOH
  6. concentrationconcentrated to the HCl salt as a yellow solid, 20 mg, 0.052 mmol, 26%