反应 #1827

反应方程式

NaCl

Hydrazine hydrate

KOH

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

HCl

→

oil

收率 87.6%

4-(3-thienyl)butyric acid

收率 87.6%

溶剂

ethylene glycol

反应条件

后处理

1. 1
   温度This solution was heated
2. 2
   温度at reflux for 6 hours
3. 3
   其他the crude reaction mixture
4. 4
   萃取extracted with ether (3×70 mL)
5. 5
   干燥The combined organic extracts were dried over Na2SO4
6. 6
   浓缩concentrated, in vacuo

实验过程

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.

来源