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
- 90 °C
PROCEDURE
实验过程
6-(Chloromethyl)-N-[6-{6-chloro-5-[(methylsulfonyl)amino]-3-pyridinyl}-1-(phenylsulfonyl)-1H-indazol-4-yl]-2-pyridinecarboxamide (50 mg, 0.079 mmol) and 2-methyl-1-(1-methylethyl)piperazine (0.5 ml, 0.047 mmol) were placed in a vial and heated in a microwave at 90° C. for 15 min. The amine was blown off under a stream of nitrogen to give an orange gum which was suspended in IPA (2 ml) and 2M NaOH (1 ml) was added. The mixture was stirred at room temperature for 2 hours then neutralised with 2M HCl (aq.) and the solvent was blown off under a stream of nitrogen. The residue was dissolved in DMSO (2 ml) (insoluble salt was filtered off through a filter tube) and purified by MDAP (Method E). The product-containing fractions were concentrated under a stream of nitrogen to give a white solid which was freeze dried to afford the title compound as a white solid (14 mg).
WORKUP
后处理
- customto give an orange gum which
- custompurified by MDAP (Method E)
- concentrationThe product-containing fractions were concentrated under a stream of nitrogen
- customto give a white solid which
- customdried