반응 #1827

반응 방정식

NaCl

Hydrazine hydrate

KOH

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

HCl

→

oil

수율 87.6%

4-(3-thienyl)butyric acid

수율 87.6%

용매

ethylene glycol

반응 조건

후처리

1. 1
   온도This solution was heated
2. 2
   온도at reflux for 6 hours
3. 3
   기타the crude reaction mixture
4. 4
   추출extracted with ether (3×70 mL)
5. 5
   건조The combined organic extracts were dried over Na2SO4
6. 6
   농축concentrated, in vacuo

실험 절차

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.

출처