تفاعل #1827

معادلة التفاعل

NaCl

Hydrazine hydrate

KOH

2-[2-oxo-2-(3-thienyl) ethyl]malonic acid

HCl

→

oil

المردود 87.6%

4-(3-thienyl)butyric acid

المردود 87.6%

المذيبات

ethylene glycol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThis solution was heated
2. 2
   درجة الحرارةat reflux for 6 hours
3. 3
   أخرىthe crude reaction mixture
4. 4
   استخلاصextracted with ether (3×70 mL)
5. 5
   تجفيفThe combined organic extracts were dried over Na2SO4
6. 6
   تركيزconcentrated, in vacuo

الإجراء التجريبي

Hydrazine hydrate (1.3 mL, 1.34 g, 26.8 mmol) was added dropwise to a solution of KOH (3.54 g, 63 mmol) and 2-[2-oxo-2-(3-thienyl) ethyl]malonic acid 8(c) (4.00 g, 17.5 mmol) in ethylene glycol (30 mL). This solution was heated at reflux for 6 hours. After cooling to room temperature, the crude reaction mixture was poured into a mixture of 6N HCl (50 mL) and ice (200 g). This aqueous mixture was saturated with NaCl, then extracted with ether (3×70 mL). The combined organic extracts were dried over Na2SO4 and concentrated, in vacuo, to provide an orange oil (2.61 g) of sufficient purity to be employed in the subsequent reaction without any further purification.

المصدر