HRID434555

反应详情

EQUATION

反应方程式

HRID 434555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.4 g of N-benzo[b]furan-7-yl-N'-2-hydroxyethylthiourea in 300 ml of ethanol are boiled under reflux and are treated with a solution of 1.12 g of sodium in 25 ml of ethanol. The hot mixture is treated with 8.1 g of mercury(II) acetate over 1/2 minute, refluxed for 15 minutes and then filtered. The filtrate is evaporated to dryness. The residue is partitioned between 40 ml of 1 N hydrochloric acid and 40 ml of methylene chloride. The aqueous phase is treated with active charcoal, filtered and made alkaline with concentrated ammonia solution. The resultant precipitate is filtered, dried and recrystallised from ethyl acetate to give the title compound in free base form. M.Pt. 124°-6°.

WORKUP

后处理

  1. temperatureunder reflux
  2. temperaturerefluxed for 15 minutes
  3. filtrationfiltered
  4. customThe filtrate is evaporated to dryness
  5. customThe residue is partitioned between 40 ml of 1 N hydrochloric acid and 40 ml of methylene chloride
  6. additionThe aqueous phase is treated with active charcoal
  7. filtrationfiltered
  8. filtrationThe resultant precipitate is filtered
  9. customdried
  10. customrecrystallised from ethyl acetate