تفاعل #1492085

معادلة التفاعل

HCl

1,2,3,4-tetrahydro-benzo[b]azepin-5-one

hydrazine monohydrate

KOH

→

compound 6

المردود 47.8%

2,3,4,5-Tetrahydro-1H-benzo[b]azepine

المردود 47.8%

المذيبات

diethylene glycol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةto reflux for 6 hr under a N2 atmosphere
3. 3
   درجة الحرارةAfter cooling
4. 4
   workup.ADDITIONthe reaction was poured onto ice-cold water
5. 5
   استخلاصextracted with EtOAc
6. 6
   غسيلAll the organics were washed with water and saturated NaCl
7. 7
   تجفيفDried over MgSO4
8. 8
   ترشيحfiltered
9. 9
   تركيزconcentrated

الإجراء التجريبي

A mixture of 1,2,3,4-tetrahydro-benzo[b]azepin-5-one (5) (1.58 g, 9.80 mmol), hydrazine monohydrate (1.92 mL, 40.0 mmol), and KOH (3.3 g, 58.8 mmol) in diethylene glycol (50 mL) was heated to reflux for 6 hr under a N2 atmosphere. After cooling, the reaction was poured onto ice-cold water, neutralized with 1N HCl, and extracted with EtOAc. All the organics were washed with water and saturated NaCl. Dried over MgSO4, filtered, and concentrated to yield compound 6 (0.69 g). This crude material was used in the next step with out further purification.

المصدر