HRID85068

反应详情

EQUATION

反应方程式

HRID 85068 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

3-(1H-indol-5-yl)-5-(4-((3-methylpiperazin-1-yl)methyl)phenyl)-1-tosyl-1H-pyrrolo[2,3-b]pyridine (50 mg) was suspended in 1 mL dichloromethane and 1 mL of methanol and treated with triethylamine (100 mL) and acetic anhydride (20 μL) and stirred for one hour. The mixture was concentrated in vacuo, taken up in EtOAc and washed with water and brine and dried over MgSO4. The residue was suspended in methanol and treated with 5 N NaOH and heated at 50° C. for one hour. The mixture was diluted with dichloromethane and washed with water and brine, dried over MgSO4 and purified by MPLC silica gel chromatography (0-20% MeOH in DCM) to yield an analytical sample (464 M+H).

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. additiontreated with 5 N NaOH
  5. additionThe mixture was diluted with dichloromethane
  6. washwashed with water and brine
  7. dry with materialdried over MgSO4
  8. custompurified by MPLC silica gel chromatography (0-20% MeOH in DCM)
  9. customto yield an analytical sample (464 M+H)