تفاعل #1768902

معادلة التفاعل

Acetic anhydride

8,9-dihydro-7-[(hydroxy)(2-methylpridin-3-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one

→

8,9-dihydro-10-methyl-7-[(2-methylpyridin-3-yl)methylene]pyrido[1,2-a]indol-6(7H)-one

المذيبات

pyridine

ظروف التفاعل

المعالجة

1. 1
   أخرىthe solution was evaporated in vacuo
2. 2
   workup.ADDITIONThe residue was diluted with chloroform
3. 3
   غسيلwashed with brine
4. 4
   تجفيفdried over anhydrous magnesium sulfate
5. 5
   أخرىevaporated in vacuo
6. 6
   workup.DISSOLUTIONThe residue and 1,8-diazabicyclo[5.4.0]undec-7-ene (1.27 g) were dissolved in toluene (30 ml)
7. 7
   workup.STIRRINGThe solution was stirred at 60° C. for 2 hours
8. 8
   أخرىevaporated in vacuo
9. 9
   أخرىThe residue was crystallized from ethyl acetate

الإجراء التجريبي

Acetic anhydride (2.24 g) was added to a solution of 8,9-dihydro-7-[(hydroxy)(2-methylpridin-3-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (1.35 g, a mixture of the isomers A and B) in pyridine (20 ml). After being stirred at 60° C. for 2 hours, the solution was evaporated in vacuo. The residue was diluted with chloroform, washed with brine, dried over anhydrous magnesium sulfate, and evaporated in vacuo. The residue and 1,8-diazabicyclo[5.4.0]undec-7-ene (1.27 g) were dissolved in toluene (30 ml). The solution was stirred at 60° C. for 2 hours and evaporated in vacuo. The residue was crystallized from ethyl acetate to give 8,9-dihydro-10-methyl-7-[(2-methylpyridin-3-yl)methylene]pyrido[1,2-a]indol-6(7H)-one (0.92 g).

المصدر