تفاعل #216680

معادلة التفاعل

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

المردود 65.4%

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

المردود 65.4%

المذيبات

dioxane

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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.

المصدر