HRID410354

反应详情

EQUATION

反应方程式

HRID 410354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

To a solution of 1-[3-(4-fluoro-phenoxy)-propyl]-1,3-dihydro-benzoimidazol-2-ylideneamine (2.0 g, 7.01 mmol) in 2-butanone (25 ml) at rt was added 2-chloro-5-chloromethyl-pyridine (2.27 g, 14.0 mmol) followed by NaBr (0.715 g, 7.01 mmol). The reaction was heated to 90° C. where it was maintained for 4 d. After this time, the suspension was cooled to rt and filtered. The collected solid was washed with additional 2-butanone and then dried to give 1-(6-chloro-pyridin-3-ylmethyl)-3-(3-phenoxy-propyl)-1,3-dihydro-benzoimidazol-2-ylideneamine, hydrochloride salt (1.6 g, 51%) which was used without further purification. HPLC-MS 411, 413 [M+1]+.

WORKUP

后处理

  1. temperaturewas maintained for 4 d
  2. temperatureAfter this time, the suspension was cooled to rt
  3. filtrationfiltered
  4. washThe collected solid was washed with additional 2-butanone
  5. customdried