反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 3-(2-bromoacetyl)benzo[b]furan (36.9 g), 2-imidazolidinethione (15.75 g), ethanol (600 ml) and acetic acid (400 ml) was heated under reflux for 21 hours then allowed to cool to ambient temperature. The resulting solid was collected by filtration, washed with ether (500 ml), and dissolved in hot methanol (500 ml). Charcoal (2 g) was added and the hot mixture was stirred for a few minutes, then filtered and allowed to cool to ambient temperature. The resulting solid was collected by filtration, ground to a fine powder, and dried in vacuo at 80° C. to give 3-(benzo[b]furan-3-yl)-5,6-dihydroimidazo[2,1-b]thiazole monohydrobromide 0.7 hydrate as an off-white solid (28.1 g), m.p. 251°-254.50C.
WORKUP
后处理
- temperaturewas heated
- temperatureunder reflux for 21 hours
- filtrationThe resulting solid was collected by filtration
- washwashed with ether (500 ml)
- dissolutiondissolved in hot methanol (500 ml)
- additionCharcoal (2 g) was added
- filtrationfiltered
- temperatureto cool to ambient temperature
- filtrationThe resulting solid was collected by filtration, ground to a fine powder
- customdried in vacuo at 80° C.