HRID351826

反应详情

EQUATION

反应方程式

HRID 351826 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[(3-Cyclopropyl-1,2,4-oxadiazol-5-yl)methyl]phthalimide (104 g, 387 mmol) was dissolved in 1,2-dichloroethane (500 mL), N-methylhydrazine (22.4 mL, 426 mmol) was added and the solution was refluxed for 5 h. The suspension was cooled in ice, the precipitate (2-methyl-2,3-dihydro-phthalazine-1,4-dione) was filtered off and washed with 1,2-dichloroethane (100 mL). The filtrate was evaporated and the residue distilled at 70° C./0.4 mbar (bath-T 100-150° C). Yield: 39.3 g (73%). m/z 139 (M).

WORKUP

后处理

  1. temperaturethe solution was refluxed for 5 h
  2. temperatureThe suspension was cooled in ice
  3. filtrationthe precipitate (2-methyl-2,3-dihydro-phthalazine-1,4-dione) was filtered off
  4. washwashed with 1,2-dichloroethane (100 mL)
  5. customThe filtrate was evaporated
  6. distillationthe residue distilled at 70° C./0.4 mbar (bath-T 100-150° C)