HRID1528307
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
1.0 g 2-[1-(chloroacetyl)piperidin-4-yl]-5-(3,4-dimethoxyphenyl)-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one (compound A1), 0.5 g morpholine-3,5-dione and 1.0 g K2CO3 in 20 ml of DMF is heated for 17 h at 80-100° C. The DMF is removed in vacuo and the residue dissolved in 70 ml of DCM, washed four times with 30 ml of water and 20 ml of 0.5 M H2SO4. The DCM layer is dried over MgSO4 and concentrated in vacuo. The title product is crystallized from diethyl ether.
WORKUP
后处理
- customThe DMF is removed in vacuo
- dissolutionthe residue dissolved in 70 ml of DCM
- washwashed four times with 30 ml of water and 20 ml of 0.5 M H2SO4
- dry with materialThe DCM layer is dried over MgSO4
- concentrationconcentrated in vacuo
- customThe title product is crystallized from diethyl ether