HRID351826
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturethe solution was refluxed for 5 h
- temperatureThe suspension was cooled in ice
- filtrationthe precipitate (2-methyl-2,3-dihydro-phthalazine-1,4-dione) was filtered off
- washwashed with 1,2-dichloroethane (100 mL)
- customThe filtrate was evaporated
- distillationthe residue distilled at 70° C./0.4 mbar (bath-T 100-150° C)