HRID1285153

反应详情

EQUATION

反应方程式

HRID 1285153 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Alloxan hydrate (1.6 g., 0.01 mole) was dissolved in 40 ml. of ethanol by heating. 5-Bromoindole (1.96 g., 0.01 mole) was added and heating near reflux continued for 15 minutes. Tlc did not indicate that reaction had occured. 1N Hydrochloric acid (10 ml.) was then added while maintaining the reaction near reflux. After 10 minutes, the reaction was concentrated to wet solids. Trituration of these wet solids with water gave the title product [3.17 g., m.p. >250° C.; Rf 0.45 (1:1 ethyl acetate:hexane/5% acetic acid); Rf 0.3 (1:5 ethyl acetate:hexane/5% acetic acid)].

WORKUP

后处理

  1. temperatureheating
  2. temperaturenear reflux
  3. customTlc did not indicate that reaction
  4. temperaturewhile maintaining
  5. customthe reaction
  6. temperaturenear reflux
  7. waitAfter 10 minutes
  8. concentrationthe reaction was concentrated to wet solids