反应详情

p-Toluenesulfonic acid monohydrate (667.33 mg) was added in one portion to a solution of N-[2-(diethylamino)ethyl]-N-(2-{[2-(4-hydroxy-2-oxo-2,3-dihydro-1,3-benzothiazol-7-yl)ethyl]amino}ethyl)-3-[2-(1-naphthyl)ethoxy]propanamide (1 g) in methanol (10 mL) producing a clear solution. This was stirred at room temperature for 30 mins then the solvent was removed in vacuo. The residue was stirred in diethyl ether (20 mL) at room temperature for 16 h then the solvent was removed and methyl t-butyl ether (20 mL) was added. This mixture was then stirred at room temperature for 16 h before the resulting solid was collected by filtration and washed with methyl t-butyl ether (5 mL). The title compound was dried in vacuo at room temperature for 16 h to leave the title compound as an amorphous solid (1.18 g).

1. customproducing a clear solution
2. customthe solvent was removed in vacuo
3. stirringThe residue was stirred in diethyl ether (20 mL) at room temperature for 16 h
4. customthe solvent was removed
5. additionmethyl t-butyl ether (20 mL) was added
6. stirringThis mixture was then stirred at room temperature for 16 h before the resulting solid
7. filtrationwas collected by filtration
8. washwashed with methyl t-butyl ether (5 mL)
9. dry with materialThe title compound was dried in vacuo at room temperature for 16 h