HRID621552

反应详情

EQUATION

反应方程式

HRID 621552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

20.0 grams of 6-chloro-7-hydroxy-3,4-dihydrocarbostyril and 3.7 g of sodium hydroxide are mixed with 100 ml of methanol and stirred for 3 hours, then 150 ml of epichlorohydrin is added thereto and heated for 5 hours under refluxing conditions. After the reaction is completed, the reaction mixture is concentrated under reduced pressure to dryness. The residue thus obtained is mixed with 100 ml of 2N-sodium hydroxide and stirred well. The insoluble matter is separated by filtration, washed with water and dried. The crude crystals thus obtained are recrystallized from methanol-ethanol to obtain 19.7 g of 6-chloro-7-(2,3-epoxypropoxy)-3,4-dihydrocarbostyril in the form of colorless crystals with a melting point of 190°-192° C.

WORKUP

后处理

  1. temperatureheated for 5 hours under refluxing conditions
  2. concentrationthe reaction mixture is concentrated under reduced pressure to dryness
  3. customThe residue thus obtained
  4. stirringstirred well
  5. customThe insoluble matter is separated by filtration
  6. washwashed with water
  7. customdried
  8. customThe crude crystals thus obtained
  9. customare recrystallized from methanol-ethanol