HRID538696

反应详情

EQUATION

反应方程式

HRID 538696 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe DMF is removed in vacuo
  2. dissolutionthe residue dissolved in 70 ml of DCM
  3. washwashed four times with 30 ml of water and 20 ml of 0.5 M H2SO4
  4. dry with materialThe DCM layer is dried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe title product is crystallized from diethyl ether