تفاعل #51824

معادلة التفاعل

1-(2,4-dichlorophenyl)-4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]-pyridine

sodium hydrogen-carbonate

→

1-(2,4-dichlorophenyl)-4-(4-oxopiperidin-1-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]pyridine

المردود 81.6%

المذيبات

hydrochloric acid

tetrahydrofuran

hydrochloric acid

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter completion of the reaction
2. 2
   استخلاصextracted three times with ethyl acetate
3. 3
   تجفيفThe combined organic layer was dried over anhydrous sodium sulfate
4. 4
   ترشيحafter which the desiccating agent was filtered off
5. 5
   تركيزthe filtrate was concentrated under reduced pressure
6. 6
   أخرىThe crystals thus obtained
7. 7
   غسيلwere washed with ethyl acetate

الإجراء التجريبي

After 1-(2,4-dichlorophenyl)-4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]-pyridine (5.21 g) was stirred in a mixture of 4 M hydrochloric acid (60 mL) and tetrahydrofuran (60 mL) at room temperature for 2.5 hours, 6 M hydrochloric acid (30 mL) was added thereto and the resulting mixture was stirred overnight. After completion of the reaction, the reaction mixture was poured into a saturated aqueous sodium hydrogen-carbonate solution and extracted three times with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate, after which the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The crystals thus obtained were washed with ethyl acetate to obtain 1-(2,4-dichlorophenyl)-4-(4-oxopiperidin-1-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]pyridine (3.83 g).

المصدر