反应 #83032

反应方程式

methyl isothiocyanate

5-(2-aminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine

→

5-(2-methylaminothiocarbonylaminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine

溶剂

ethanol

反应条件

后处理

1. 1
   温度The mixture was refluxed for 3 hours
2. 2
   workup.DISTILLATIONThe reaction mixture was subjected to vacuum distillation
3. 3
   其他to remove ethanol
4. 4
   workup.ADDITIONThe residue was mixed with a saturated aqueous sodium hydrogencarbonate solution
5. 5
   萃取followed by extraction with ethyl acetate
6. 6
   干燥The organic layer was dried over magnesium sulfate
7. 7
   workup.DISTILLATIONsubjected to vacuum distillation
8. 8
   其他to remove the solvent
9. 9
   其他The residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol =50/1)

实验过程

0.13 ml of methyl isothiocyanate was added to 20 ml of a suspension of 0.5 g of 5-(2-aminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine in ethanol. The mixture was refluxed for 3 hours. The reaction mixture was subjected to vacuum distillation to remove ethanol. The residue was mixed with a saturated aqueous sodium hydrogencarbonate solution, followed by extraction with ethyl acetate. The organic layer was dried over magnesium sulfate and then subjected to vacuum distillation to remove the solvent. The residue was purified by silica gel column chromatography (elutant: dichloromethane/methanol =50/1) to obtain 0.46 g of 5-(2-methylaminothiocarbonylaminoethoxy)-7-chloro-1-[2-methoxy-4-(2-chlorobenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzoazepine.

来源