反応 #2267076

反応方程式

14

6-Acetylamino-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

→

desired product 15

収率 100.0%

6-Amino-3-methyl-1-(4-nitrophenyl)-7-methoxyisochroman

収率 100.0%

溶媒

H2SO4

methanol

反応条件

後処理

1. 1
   温度After refluxing for 15 hours
2. 2
   その他the methanol was removed under reduced pressure
3. 3
   抽出followed by extraction with ethyl acetate three times
4. 4
   乾燥The combined organic phase was dried over Na2SO4
5. 5
   その他Removal of the solvent

実験手順

Solution of 14 (0.114 g, 0.32 mmol) in 5 ml of 4N H2SO4 and 5 ml of methanol was heated to reflux. After refluxing for 15 hours, the methanol was removed under reduced pressure. The remaining aqueous solution was neutralized with NaHCO3 to pH 9, followed by extraction with ethyl acetate three times. The combined organic phase was dried over Na2SO4. Removal of the solvent afforded the desired product 15 (100 mg, 100%) which was used directly for next step.

出典