HRID1651549

反应详情

EQUATION

反应方程式

HRID 1651549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

After 2.00 g (6.60 mmol) of 4-[(4-chlorophenyl)-2-pyridylmethoxy]piperidine and 2.39 g (8.17 mmol) of 2-(2-bromoethylthio)-5-chlorobenzoxazole were dissolved in 10 ml of dioxane, 1.10 g (7.96 mmol) of potassium carbonate was added to the mixed solution, and the mixture was stirred at an oil bath temperature of 75° to 80° C. for 6 hours. After the reaction, the insolubles were filtered off, and the filtrate was concentrated under reduced pressure. The residue was separated by silica gel column chromatography with a mixed solution of chloroform and methanol in the volume ratio 50:1 as an eluent. The desired fraction was concentrated to give 1.83 g (54%) of 5-chloro-2-[2-[4-[(4-chlorophenyl)-2-pyridylmethoxy]-1-piperidyl]ethylthio]benzoxazole as an oily product.

WORKUP

后处理

  1. customAfter the reaction
  2. filtrationthe insolubles were filtered off
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was separated by silica gel column chromatography with a mixed solution of chloroform and methanol in the volume ratio 50:1 as an eluent
  5. concentrationThe desired fraction was concentrated