HRID635372

反应详情

EQUATION

反应方程式

HRID 635372 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 1-[1-(benzo[b]thiophen-2-yl)cyclobutyl]-2-bromoethanone (0.42 g), imidazolidine-2-thione (0.14 g), ethanol (15 ml) and acetic acid (10 ml) was heated under reflux for 18 hours then allowed to cool to ambient temperature. The solvents were removed in vacuo and the residue was triturated with ether (30 ml). The resulting solid was collected by filtration, dried in vacuo at 40° C. and crystallised from ethanol. The resulting product was collected by filtration, washed with ethanol (3 ml) and dried in vacuo at 40° C. to give 3-[1-(benzo[b]thiophen-2-yl)cyclobutyl]-5,6-dihydroimidazo[2,1-b]thiazole hydrobromide as an off-white solid (0.28 g), m.p. 240-242° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. customThe solvents were removed in vacuo
  4. customthe residue was triturated with ether (30 ml)
  5. filtrationThe resulting solid was collected by filtration
  6. customdried in vacuo at 40° C.
  7. customcrystallised from ethanol
  8. filtrationThe resulting product was collected by filtration
  9. washwashed with ethanol (3 ml)
  10. customdried in vacuo at 40° C.