HRID1281659

反应详情

EQUATION

反应方程式

HRID 1281659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

40 ml of hydrazine hydrate were added to a solution of 30 g (0.15 mol) of methyl 3-nitrosalicylate in 200 ml of anhydrous tetrahydrofuran (THF). After dilution with THF, the resulting suspension was stirrable; it was refluxed for approximately 18 hours. After cooling, the batch was poured onto ice. The aqueous solution was rendered neutral by adding NaOH solution. The crystals which precipitated were filtered off and washed with water. After drying, 27 g (90%) of the title compound were obtained.

WORKUP

后处理

  1. temperatureit was refluxed for approximately 18 hours
  2. temperatureAfter cooling
  3. additionthe batch was poured onto ice
  4. customThe crystals which precipitated
  5. filtrationwere filtered off
  6. washwashed with water
  7. customAfter drying