反应 #499166

反应方程式

4-(3,4-dichlorophenyl)-2-[2-(4-methylpiperazin-1-yl)-benzylidene]-thiomorpholin-3-one

a-chloroethyl chloroformate

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title compound

4-(3,4-Dichlorophenyl)-2-(2-piperazin-1-ylbenzylidene)-thiomorpholin-3-one

溶剂

1,2-dichloroethane

反应条件

后处理

1. 1
   温度refluxed overnight
2. 2
   其他The solvent was then removed in vacuo and 10 mL of methanol
3. 3
   workup.ADDITIONwas added
4. 4
   温度refluxed for 30 minutes
5. 5
   其他removal of the solvent
6. 6
   萃取the residue was extracted into methylene chloride
7. 7
   洗涤washed with saturated aqueous sodium carbonate (Na2CO3) and saturated brine
8. 8
   干燥dried with magnesium sulfate
9. 9
   浓缩concentrated to a foam

实验过程

Under a nitrogen atmosphere, a mixture of 4-(3,4-dichlorophenyl)-2-[2-(4-methylpiperazin-1-yl)-benzylidene]-thiomorpholin-3-one (338 mg, 0.756 mmol) in 9 mL of anhydrous 1,2-dichloroethane was treated with a-chloroethyl chloroformate (98 μL 0.907 mmol) and refluxed overnight. The solvent was then removed in vacuo and 10 mL of methanol was added and refluxed for 30 minutes. Following removal of the solvent, the residue was extracted into methylene chloride and washed with saturated aqueous sodium carbonate (Na2CO3) and saturated brine, dried with magnesium sulfate and concentrated to a foam. Flash chromatography using triethyl amine/methanol/ethyl acetate (1:2:97) gave the purified free base of the title compound.

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