HRID1182846

反应详情

EQUATION

反应方程式

HRID 1182846 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

397 mg (6.4 mmol) ethylene glycol was added to 115 mg (4.8 mmol) NaH in 20 ml THF and the mixture was stirred at room temperature for 30 min. Then, 500 mg (1.6 mmol) 7-bromo-2,4-dichloro-5H-pyrimido[5,4-b]indole (Example 4) was added and the mixture was refluxed for 5 h. Thereafter, the solvent was removed and the residue was taken up in acetic ester and washed with saturated NaCl solution, dried over Na2SO4 and filtrated. Having removed the solvent, 450 mg (88%) 2-(7-bromo-2-chloro-5H-pyrimido[5,4-b]indol-4-yloxy)ethanol was obtained. ESI-MS [m/z]: 342, 344 [M+H]+

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 5 h
  2. customThereafter, the solvent was removed
  3. washwashed with saturated NaCl solution
  4. dry with materialdried over Na2SO4
  5. filtrationfiltrated
  6. customHaving removed the solvent