HRID2267303

反应详情

EQUATION

反应方程式

HRID 2267303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

1-Thiophen-2-yl-ethanone (100 mg, 0.79 mmol) was dissolved in DMF-DMA (1 mL) and heated at 100° C. for 16 h. The solution was concentrated to give a gum. This was treated with a solution of N-[2-(2-oxo-imidazolidin-1-yl)-ethyl]-guanidine hydrochloride (233 mg, 1.12 mmol) in NMP (1.5 mL), cesium carbonate (228 mg, 0.7 mmol) was added and the mixture was heated at 100° C. for 16 h. The mixture was cooled and filtered, concentrated, and purified by preparative HPLC to give the product (140 mg, 61%) as an amorphous off-white solid. MS (M+H)+ 290.

WORKUP

后处理

  1. concentrationThe solution was concentrated
  2. customto give a gum
  3. additionwas added
  4. temperaturethe mixture was heated at 100° C. for 16 h
  5. temperatureThe mixture was cooled
  6. filtrationfiltered
  7. concentrationconcentrated
  8. custompurified by preparative HPLC