HRID1378533

反应详情

EQUATION

反应方程式

HRID 1378533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

An ice cooled solution of 3-[1-(1-methyl-piperidin-4-yl)-1H-indol-3-yl]-4-(1-methyl-1H-indol-3-yl)-pyrrole-2,5-dione (70 g, 0.16 mol) in ethyl acetate (4 L) was saturated with gaseous hydrogen chloride for 3 hours. The precipitate formed was isolated by suction filtration, suspended in methanol (3 L) and stirred for 30 minutes. The mixture turned into a homogenous slurry, which was concentrated and treated with ether (500 mL). The title compound crystallized and was collected by suction filtration. The filter was vacuum dried over night (100° C./0.1 mm. Yield 70 g (92% of theory). M.Pt.: 280°-282° C.

WORKUP

后处理

  1. customThe precipitate formed
  2. customwas isolated by suction filtration
  3. concentrationwas concentrated
  4. additiontreated with ether (500 mL)
  5. customThe title compound crystallized
  6. filtrationwas collected by suction filtration
  7. customdried over night (100° C./0.1 mm