HRID490117
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture was purified by RP HPLC (C18, CH3CN/H2O 0.1% TFA)
- additionthe pure fractions were poured into ethyl acetate/0.5 N NaOH
- dry with materialThe organic phase was dried over sodium sulfate
- concentrationconcentrated to a yellow solid which
- dissolutionwas dissolved in 1N HCl in MeOH
- concentrationconcentrated to the HCl salt as a yellow solid, 20 mg, 0.052 mmol, 26%