HRID1273034

反应详情

EQUATION

反应方程式

HRID 1273034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

The title compound was prepared by adding the 3-bromo-1-perhydro-2H-pyran-2-yl-1H-indazole-5-carbonitrile (15.20 g, 49.65 mmol), ethanol (130 mL), 30% hydrogen peroxide (aqueous) (130 mL), and 6 N sodium hydroxide (aqueous) (9 mL) to a 2 liter round bottom flask. This mixture was heated at 50° C. for 1 hour, and removed from the heat to allow to cool to room temperature. The pH was adjusted to ˜3 by adding 6 N hydrochloride solution (aqueous) resulting in a precipitate. This precipitate was filtered and washed with water (15.13 g, 94%): ES-MS (m/z) 324 [M+1]+.

WORKUP

后处理

  1. customremoved from the
  2. temperatureheat
  3. temperatureto cool to room temperature
  4. additionby adding 6 N hydrochloride solution (aqueous)
  5. customresulting in a precipitate
  6. filtrationThis precipitate was filtered
  7. washwashed with water (15.13 g, 94%)