HRID656382

反应详情

EQUATION

反应方程式

HRID 656382 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

A stirred mixture of (±)-6′-carboxy-3′,4′-dihydro-1′H-spiro[imidazolidine-4,2′-naphthalene]-2,5-dione (described in Intermediate 1) (1.50 g, 5.76 mmol), and sodium azide (749 mg, 11.53 mmol) in conc. H2SO4 (30 mL) was heated to 50° C. for 2 h, then allowed to cool to ambient temperature. The mixture was adjusted to pH 8 by addition of 6 N aqueous NaOH and concentrated in vacuo to precipitate a solid. The precipitate was collected by filtration and washed extensively with H2O. Drying in vacuo afforded the title compound. MS: m/z=232 (M+1).

WORKUP

后处理

  1. temperatureto cool to ambient temperature
  2. concentrationconcentrated in vacuo
  3. customto precipitate a solid
  4. filtrationThe precipitate was collected by filtration
  5. washwashed extensively with H2O
  6. customDrying in vacuo