반응 #216680

반응 방정식

water

2-bromopropionyl bromide

2-amino-3-(2-chlorobenzoyl)-6-(3-butynyloxycarbonyl)-4,5,6,7-tetrahydro-thieno[2,3-C]pyridine

pyridine

→

intended compound

수율 65.4%

2-(2-Bromopropionylamino)-3-(2-chlorobenzoyl)-6-(3-butynyloxycarbonyl)-4,5,6,7-tetrahydro-thieno[2,3-C]pyridine

수율 65.4%

용매

dioxane

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타by dropping at 0° C
3. 3
   기타After completion of the reaction
4. 4
   추출extracted with dichloromethane
5. 5
   건조dried with anhydrous magnesium sulfate
6. 6
   workup.DISTILLATIONafter which the solvent was distilled off under reduced pressure
7. 7
   기타The resultant residue was purified by silica gel column chromatography (elution solvent: dichloromethane:hexane=1:1-1:0)

실험 절차

1.35 g of 2-amino-3-(2-chlorobenzoyl)-6-(3-butynyloxycarbonyl)-4,5,6,7-tetrahydro-thieno[2,3-C]pyridine was dissolved in 20 ml of dioxane, to which 0.33 g of pyridine was added, followed by dropping at 0° C. 0.90 g of 2-bromopropionyl bromide. After completion of the reaction, the reaction mixture was charged into water, extracted with dichloromethane and dried with anhydrous magnesium sulfate, after which the solvent was distilled off under reduced pressure. The resultant residue was purified by silica gel column chromatography (elution solvent: dichloromethane:hexane=1:1-1:0), thereby obtaining 1.19 g of the intended compound.

출처