반응 #662226

반응 방정식

methyl 9-bromo-10-fluoro-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene-4-carboxylate

→

9-bromo-10-fluoro-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene-4-carboxylic acid

수율 86.2%

용매

methanol NaOH

반응 조건

후처리

1. 1
   기타Into a 5000-mL 4-necked round-bottom flask was placed
2. 2
   온도The resulting solution was heated
3. 3
   온도to reflux for 1.5 hours
4. 4
   농축concentrated under vacuum
5. 5
   여과The precipitates were collected by filtration
6. 6
   세척washed with 1×1000 mL of water
7. 7
   기타dried

실험 절차

Into a 5000-mL 4-necked round-bottom flask was placed a solution of methyl 9-bromo-10-fluoro-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene-4-carboxylate (110 g, 313.24 mmol, 1.00 equiv) in methanol/NaOH (40%) (1000 mL). The resulting solution was heated to reflux for 1.5 hours and concentrated under vacuum. Hydrogen chloride (2 mol/L) was used to adjust the pH to 4. The precipitates were collected by filtration, washed with 1×1000 mL of water and dried to afford 91 g (86%) of 9-bromo-10-fluoro-2,5-diazatetracyclo[11.1.1.0[2,6].0[7,12]]pentadeca-3,5,7,9,11-pentaene-4-carboxylic acid as a white solid.

출처