HRID430549

反应详情

EQUATION

反应方程式

HRID 430549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Catalyst (0.10 g of 10% platinum on carbon) was added to a solution of 6-methyl-3-nitroquinolin-4-ol (1 g) in ethanol (25 mL) and ammonium hydroxide (0.5 mL). The mixture was reduced on a Parr apparatus at ambient temperature under a hydrogen atmosphere. The reaction mixture was filtered to remove the catalyst and then concentrated under vacuum. The residue was combined with water and heated. Hydrochloric acid was added dropwise until all of the solid had dissolved. Activated carbon was added to the solution. The mixture was filtered. Hydrochloric acid (2 mL of 12N) was added to the filtrate. This recrystallization was run three times to provide 0.50 g of 3-amino-6-methylquinolin-+4ol hydrochloride, m.p. >310° C. Analysis: Calculated for C10H10N2O.HCl: % C, 57.02; % H, 5.26; % N, 13.30; Found: % C, 56.92; % H, 5.16; % N, 13.24.

WORKUP

后处理

  1. customwas reduced on a Parr apparatus at ambient temperature under a hydrogen atmosphere
  2. filtrationThe reaction mixture was filtered
  3. customto remove the catalyst
  4. concentrationconcentrated under vacuum
  5. temperatureheated
  6. additionHydrochloric acid was added dropwise until all of the solid
  7. dissolutionhad dissolved
  8. additionActivated carbon was added to the solution
  9. filtrationThe mixture was filtered
  10. additionHydrochloric acid (2 mL of 12N) was added to the filtrate
  11. customThis recrystallization