HRID864480

反应详情

EQUATION

反应方程式

HRID 864480 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Fluorotryptamine hydrochloride (0.511 g, 2.38 mmol) was dissolved in water (9 ml). Glyoxylic acid monohydrate (0.241 g, 2.618 mmol) was added, followed by KOH (0.129 g, 2.31 mmol). The resultant solid was stirred at ambient temperature for one hour before concentrated HCl (0.6 ml) was added in one portion. The mixture was refluxed for 30 minutes, more concentrated hydrogen chloride (0.6 ml) was added and the mixture was again refluxed for 15 minutes. The mixture was cooled to room temperature and basified to pH12 using 5N sodium hydroxide. It was extracted with chloroform (4×75 ml), separated, dried over magnesium sulphate, filtered and concentrated in vacuo to yield an off-white solid.

WORKUP

后处理

  1. additionwas added in one portion
  2. temperatureThe mixture was refluxed for 30 minutes
  3. temperaturethe mixture was again refluxed for 15 minutes
  4. extractionIt was extracted with chloroform (4×75 ml)
  5. customseparated
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto yield an off-white solid