HRID1360183

反应详情

EQUATION

反应方程式

HRID 1360183 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl N-[(4-chloro-1H-pyrrolo[2,3-b]pyridin-5-yl)carbonyl]glycinate (167 mg) in chloroform (5 ml) was added diphosphorus pentoxide (886 mg) under ambient temperature, and the mixture was refluxed for 18 hours. The reaction solution was cooled and added to saturated aqueous sodium hydrogencarbonate. The reaction solution was extracted with ethyl acetate. The organic layer was washed with water. The organic layer was dried over magnesium sulfate and filtered. The filtrate was concentrated under reduced pressure. The residue was purified by thin-layer silica gel column chromatography (chloroform:methanol=15:1) to obtain 4-chloro-5-(5-methoxy-1,3-oxazol-2-yl)-1H-pyrrolo[2,3-b]pyridine (45 mg) as a yellowish white solid.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 18 hours
  2. temperatureThe reaction solution was cooled
  3. extractionThe reaction solution was extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customThe residue was purified by thin-layer silica gel column chromatography (chloroform:methanol=15:1)