反応 #662226

反応方程式

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

収率 86.2%

溶媒

methanol NaOH

反応条件

後処理

1. 1
   その他Into a 5000-mL 4-necked round-bottom flask was placed
2. 2
   温度The resulting solution was heated
3. 3
   温度to reflux for 1.5 hours
4. 4
   濃縮concentrated under vacuum
5. 5
   ろ過The precipitates were collected by filtration
6. 6
   洗浄washed with 1×1000 mL of water
7. 7
   その他dried

実験手順

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.

出典