HRID346793

反应详情

EQUATION

反应方程式

HRID 346793 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a water separator, indole (50 g, 0.43 mol.), ε-caprolactone (oxepan-2-one, 55.9 g, 0.49 mol.), potassium hydroxide (35.9 g, 0.64 mol.) in p-cymene (1-isopropyl-4-methylbenzene, 250 ml) were heated at boiling for 4 d, with stirring. For working up, water (200 ml) was added to the mixture, the phases were separated, and the aqueous phase was adjusted to pH 4 with 2M HCl and stored for 2 d at 4° C. in a refrigerator. The resulting solid was filtered off with suction and washed with water (3×20 ml). Recrystallisation from ether (50 ml) yielded 6-(1H-indol-3-yl)hexanoic acid in the form of a white solid having a melting point of 124–126° C. in a yield of 16.9 g.

WORKUP

后处理

  1. customthe phases were separated
  2. waitstored for 2 d at 4° C. in a refrigerator
  3. filtrationThe resulting solid was filtered off with suction
  4. washwashed with water (3×20 ml)
  5. customRecrystallisation from ether (50 ml)