HRID1695780

反应详情

EQUATION

反应方程式

HRID 1695780 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customto give an orange gum which
  2. custompurified by MDAP (Method E)
  3. concentrationThe product-containing fractions were concentrated under a stream of nitrogen
  4. customto give a white solid which
  5. customdried