反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A suspension of 2-[2-(2-amino-thiazol-4-yl)-ethyl]isoindole-1,3-dione hydrobromide (25.7 g, 72.6 mmol, 1 eq.) in water (125 mL) was treated with 62% hydrobromic acid in water (125 mL). The resulting suspension was then refluxed (oil bath temperature=120° C.), under N2 for 18 hours. The resulting orange homogeneous reaction mixture was allowed to cool down to r.t. (fast precipitation of a beige solid occurred). The resulting suspension was filtered and the filter cake (phthalic acid) was washed with water. The obtained orange homogeneous filtrate was then concentrated in vacuo. The remaining water was finally removed by co-evaporation with toluene (repeated several times) and the obtained residue was further dried under hv to give the dihydrobromide salt of the title compound as an orange solid. The product was used without further purification.
WORKUP
后处理
- temperatureto cool down to r.t. (
- customfast precipitation of a beige solid
- filtrationThe resulting suspension was filtered
- washthe filter cake (phthalic acid) was washed with water
- concentrationThe obtained orange homogeneous filtrate was then concentrated in vacuo
- customThe remaining water was finally removed by co-evaporation with toluene (repeated several times)
- customthe obtained residue was further dried under hv