HRID610478

反应详情

EQUATION

反应方程式

HRID 610478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 4-chloro-α,α-dimethyl-1H-imidazo[4,5-c]quinoline-1-ethanol (1.0 g, 3.6 mmole, U.S. Pat. No. 4,689,338 Example 189 Part D) in hydrazine (3 mL, 6.9 mmole) was heated on a steam bath for 1 hour then diluted with water. The resulting precipitate was isolated by filtration. The solid was dissolved in a mixture of acetic acid (2 mL) and water (15 mL) then combined with a solution of sodium nitrite (0.5 g) in water. The resulting precipitate was isolated by filtration, washed with water and dried to provide 0.71 g of α,α-dimethyl-6H-imidazo [4,5-c]tetrazolo[1,5-a]quinoline-6-ethanol as a white solid, m.p. 246-247° C. (shrunk at 230° C.). Analysis: Calculated for C14H14N6O: % C, 59.56; % H, 5.00; % N, 29.77; Found: % C, 59.45; % H, 5.06; % N, 29.51.

WORKUP

后处理

  1. customThe resulting precipitate was isolated by filtration
  2. customThe resulting precipitate was isolated by filtration
  3. washwashed with water
  4. customdried