تفاعل #684950

معادلة التفاعل

compound

(4-Butylphenyl)(1-isoquinolyl)ketone

hydrazine monohydrate

potassium hydroxide

→

title compound

المردود 55.3%

1-(4-Butylbenzyl)Isoquinoline

المردود 55.3%

المذيبات

diethylene glycol

ظروف التفاعل

المعالجة

1. 1
   workup.WAITat 200° C. for 1 hour
2. 2
   درجة الحرارةThe mixture was cooled to room temperature
3. 3
   استخلاصthis was extracted with ethyl acetate
4. 4
   غسيلThe extract was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulfate
6. 6
   تركيزconcentrated under reduced pressure
7. 7
   أخرىThe residue was purified by silica gel column chromatography

الإجراء التجريبي

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).

المصدر