HRID1748568

反应详情

EQUATION

反应方程式

HRID 1748568 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 1-(5-acetylpyridin-2-yl)pyrrole-3-carboxylic acid tert-butyl ester (380 mg) in dichloromethane (5 ml) were added trifluoroacetic acid (3 ml) and water (0.3 ml), and stirred at room temperature. After completion of the reaction, the solvent was evaporated in vacuo, to the residue was added water, 1 N aqueous solution of sodium hydroxide was added thereto under ice-cooling to adjust the mixture to pH 10, diethyl ether was added thereto, and the aqueous layer was separated. To the aqueous layer was added concentrated hydrochloric acid under ice-cooling, the precipitated solid was collected by filtration, and dried at 60° C. under air blow to give the titled compound (300 mg) as a white solid. MS (ESI) m/z: 231

WORKUP

后处理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated in vacuo, to the residue
  3. additionwas added water, 1 N aqueous solution of sodium hydroxide
  4. additionwas added
  5. temperatureunder ice-cooling
  6. additionwas added
  7. customthe aqueous layer was separated
  8. additionTo the aqueous layer was added concentrated hydrochloric acid under ice-
  9. temperaturecooling
  10. filtrationthe precipitated solid was collected by filtration
  11. customdried at 60° C. under air blow