HRID1164496

反应详情

EQUATION

反应方程式

HRID 1164496 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 125.25 g (0.395 mole) of N-[6-(2-methyl-1,3-dioxolan-2-yl)hexyl]phthalimide, 23 ml of 85% hydrazine hydrate, and 370 ml of 95% ethanol was refluxed for four hours, cooled, filtered and stripped. The residue was mixed with 500 ml of water, basified with 2 N NaOH solution and extracted with methylene chloride. The organic layer was separated, dried over anhydrous potassium carbonate, filtered, and stripped to an orange oil. This material was distilled to give 35.70 g (64%) of clear oil bp 80°-83° (0.100 mm).

WORKUP

后处理

  1. temperaturewas refluxed for four hours
  2. temperaturecooled
  3. filtrationfiltered
  4. additionThe residue was mixed with 500 ml of water
  5. extractionextracted with methylene chloride
  6. customThe organic layer was separated
  7. dry with materialdried over anhydrous potassium carbonate
  8. filtrationfiltered
  9. distillationThis material was distilled