HRID277990

反应详情

EQUATION

反应方程式

HRID 277990 的结构方程式

PROCEDURE

实验过程

To a mixture of 5-methoxy-4-aza-1H-indole(7.0 g, 47 mmol) and potassium hydroxide (9.2 g, 165 mmol) in 350 mL of methanol was added 1-methyl-4-piperidone (9.86 mL, 80 mmol) in one portion. The reaction was heated at reflux temperature overnight, and cooled to room temperature. The resulting precipitate was collected, and the filtrate was concentrated to a minimal volume. A second crop of crystals was collected, washed with cold methanol, and combined with the previous crop to afford 9.0 g (79%) of the title compound. MS(m/e): 243 (M+). EA calculated for C14H17N3O: C, 69.11; H, 7.04; N, 17.27. Found: C, 69.22; H, 7.13; N, 17.47.

WORKUP

后处理

  1. temperatureThe reaction was heated
  2. temperatureat reflux temperature overnight
  3. customThe resulting precipitate was collected
  4. concentrationthe filtrate was concentrated to a minimal volume
  5. customA second crop of crystals was collected
  6. washwashed with cold methanol