反応 #2267080

反応方程式

22

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

acetic hydrazide

→

desired product 23

収率 86.5%

2′-Acetylamino-6′-(2-hydroxypropyl)-3′-methoxy-4-nitrobenzophenone acetylhydrazone

収率 86.5%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The resulting solution was refluxed for 3 hours
2. 2
   その他The solvent was removed under reduced pressure
3. 3
   workup.ADDITIONThe residue was treated with NaHCO3
4. 4
   抽出extracted with ethyl acetate
5. 5
   洗浄The combined organic phases were washed with brine
6. 6
   乾燥dried over Na2SO4
7. 7
   その他Removal of the solvent

実験手順

To a solution of 22 (1.7 g) in 25 ml of ethanol was added acetic hydrazide (0.5 g) and 2 drops of concentrated HCl. The resulting solution was refluxed for 3 hours. The solvent was removed under reduced pressure. The residue was treated with NaHCO3, and extracted with ethyl acetate. The combined organic phases were washed with brine, dried over Na2SO4. Removal of the solvent gave the desired product 23 (1.25 g).

出典