HRID722270

反应详情

EQUATION

反应方程式

HRID 722270 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Isoamyl nitrite (15 ml, 108 mmol) was added to a solution of indan-1,2-dione (12 g, 90 mmol) in MeOH (380 ml) at 45° C. followed by concentrated HCl (12 ml) dropwise over 5 minutes. The reaction mixture was stirred for 3 hours at room temperature. Excess isoaamyl nitrite (1 ml) and concentrated HCl (1 ml) was added and the suspension stirred for a further 15 minutes. On cooling to room temperature a white precipitate formed. The precipitate was filtered off and washed with cold MeOH (40 ml) followed by Et2O (40 ml) to afford indan-1,2-dione-2-oxime (6.2 g, 43%) as a white solid.

WORKUP

后处理

  1. stirringthe suspension stirred for a further 15 minutes
  2. temperatureOn cooling to room temperature a white precipitate
  3. customformed
  4. filtrationThe precipitate was filtered off
  5. washwashed with cold MeOH (40 ml)