تفاعل #1372603

معادلة التفاعل

methanesulfonyl chloride

reactin

sodium chloride

6-hydroxy-7-(3-chloropropionyl)-3,4-dihydrocarbostyril

→

6-methylsulfonyloxy-7-(3-chloropropionyl)-3,4-dihydrocarbostyril

المذيبات

dimethylformamide

pyridine

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added to the mixture
2. 2
   استخلاصextracted with chloroform
3. 3
   غسيلThe chloroform layer was washed with water
4. 4
   أخرىdried
5. 5
   أخرىchloroform was removed by distillation under a reduced pressure
6. 6
   أخرىto obtain a residue
7. 7
   أخرىThe residue was crystallized
8. 8
   workup.ADDITIONby adding 80 ml of hexane
9. 9
   أخرىto obtain crude crystals
10. 10
    ترشيحThe crude materials were collected by filtration
11. 11
    أخرىwere recrystallized from ethanol

الإجراء التجريبي

5.06 Grams of 6-hydroxy-7-(3-chloropropionyl)-3,4-dihydrocarbostyril and 1.8 g of anhydrous pyridine were mixed with 50 ml of dimethylformamide. Then the mixture was cooled with ice and 2.5 g of methanesulfonyl chloride was added to the mixture and stirred at a room temperature for 3 hours. The reactin mixture was poured into 100 ml of a saturated sodium chloride solution and extracted with chloroform. The chloroform layer was washed with water, dried and chloroform was removed by distillation under a reduced pressure to obtain a residue. The residue was crystallized by adding 80 ml of hexane to obtain crude crystals. The crude materials were collected by filtration and were recrystallized from ethanol to obtain 4.5 g of 6-methylsulfonyloxy-7-(3-chloropropionyl)-3,4-dihydrocarbostyril in white crystals.

المصدر