反応 #684950

反応方程式

compound

(4-Butylphenyl)(1-isoquinolyl)ketone

hydrazine monohydrate

potassium hydroxide

→

title compound

収率 55.3%

1-(4-Butylbenzyl)Isoquinoline

収率 55.3%

溶媒

diethylene glycol

反応条件

後処理

1. 1
   workup.WAITat 200° C. for 1 hour
2. 2
   温度The mixture was cooled to room temperature
3. 3
   抽出this was extracted with ethyl acetate
4. 4
   洗浄The extract was washed with water
5. 5
   乾燥dried over anhydrous magnesium sulfate
6. 6
   濃縮concentrated under reduced pressure
7. 7
   その他The residue was purified by silica gel column chromatography

実験手順

The compound of Example B3 (1.7 g, 6.0 mmol), hydrazine monohydrate (836 mg, 17 mmol), and potassium hydroxide (769 mg, 14 mmol) were added to diethylene glycol (8.5 ml), and this mixture was stirred at 80° C. for 1 hour, at 160° C. for 3.5 hours, then at 200° C. for 1 hour. The mixture was cooled to room temperature, ice water was added, and this was extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (914 mg).

出典