HRID48295

反应详情

EQUATION

反应方程式

HRID 48295 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N4-(2-methylpropyl)quinoline-3,4-diamine (5.4 g, 25 mmol) was combined with carbon disulfide (9 mL, 150 mmol) and ethanol (55 mL) and then heated at reflux on a steam bath for 2 hours. The resulting precipitate was isolated by filtration, washed with ethanol and then air dried to provide 4.4 g of crude product. A portion (1 g) was dissolved in hot dilute sodium hydroxide and then reprecipitated with acetic acid. The precipitate was isolated by filtration while still hot, washed with hexane and then air dried to provide thiazolo[4,5-c]quinoline-2-thiol as a solid, m.p. 282-284° C. Analysis: Calculated for C10H6N2S2: %C, 55.02; %H, 2.77; %N, 12.83: Found: %C, 54.96; %H, 2.69; %N, 12.74.

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux on a steam bath for 2 hours
  3. customThe resulting precipitate was isolated by filtration
  4. washwashed with ethanol
  5. customair dried
  6. customto provide 4.4 g of crude product
  7. customreprecipitated with acetic acid
  8. customThe precipitate was isolated by filtration while still hot,
  9. washwashed with hexane
  10. customair dried