HRID1288600

反应详情

EQUATION

反应方程式

HRID 1288600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of 4-methyl-1,3-indanedione (1.02g. 0.006 mole) in anhydrous ether (5 ml) at ca 10° C was added drowpwise and with stirring fuming nitric acid (2.0 ml). After 10 mins. a clear, dark solution formed followed by precipitation of a bright yellow solid. The mass was filtered and washed with 5N hydrochloric acid. Recrystallisation from water/hydrochloric acid afforded the title compound, m.p. 108°-9° C. (Found; C, 56.16; H, 3.74; N, 6.32; C10H7NO4.1 /2H2O requires; C, 56.07; H, 3.76; N, 6.54%).

WORKUP

后处理

  1. additionwas added drowpwise
  2. customa clear, dark solution formed
  3. customfollowed by precipitation of a bright yellow solid
  4. filtrationThe mass was filtered
  5. washwashed with 5N hydrochloric acid
  6. customRecrystallisation from water/hydrochloric acid