HRID648446

反应详情

EQUATION

反应方程式

HRID 648446 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

A mixture of 5.0 g of 3-cyano-2(1H)-quinolinone, 1.9 g of ammonium chloride and 2.4 g of sodium azide in 50 ml of dimethylformamide was heated at 120° C for 16 hours. The mixture was then poured into 250 ml of water and the resulting mixture was acidified to pH 2 with concentrated hydrochloric acid. The solid which formed was separated by filtration and dried. It was then dissolved in aqueous sodium hydroxide and the aqueous solution was washed with methylene chloride and filtered and the filtrate was acidified with hydrochloric acid. The light tan solid which formed was separated by filtration and dried to give 3-(IH-tetrazol-5-yl)-2(1H)-quinolinone 1/9 hydrate melting at about 301°-303° C. with decomposition.

WORKUP

后处理

  1. customThe solid which formed
  2. customwas separated by filtration
  3. customdried
  4. dissolutionIt was then dissolved in aqueous sodium hydroxide
  5. washthe aqueous solution was washed with methylene chloride
  6. filtrationfiltered
  7. customThe light tan solid which formed
  8. customwas separated by filtration
  9. customdried