HRID1070697

反应详情

EQUATION

反应方程式

HRID 1070697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of methyl (2Z,4E)-5-(5,6-dichloroindol-2-yl)-2-methoxy-2,4-pentadienoate (10 g, 30.7 mmol) and KOH (3.6 g, 64.2 mmol) in EtOH/water {fraction (1/1)} (460 ml) was refluxed for 3 h. The suspension after cooling to RT was poured into water (1.5 l), it was acidified with 2N HCl and extracted with AcOEt (2×1 l). The organic phase was washed with water and dried (MgSO4), then concentrated and the residue taken up with CH2Cl2. Filtration and drying in the oven at 50° produced 9.5 g of pure title compound (30.4 mmol, yield 99.1%), m.p.=249-250° C.

WORKUP

后处理

  1. temperaturewas refluxed for 3 h
  2. extractionextracted with AcOEt (2×1 l)
  3. washThe organic phase was washed with water
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. filtrationFiltration
  7. customdrying in the oven at 50°