海萝胶 → 4-(噻吩-3-基)丁酸

HRID 1731

反应方程式

HRID 1731 反应方程式
O.NN.[OH-].[K+].O=[C:7]([C:16]1[CH:20]=[CH:19][S:18][CH:17]=1)[CH2:8][CH:9](C(O)=O)[C:10]([OH:12])=[O:11].Cl.[Na+].[Cl-]>C(O)CO>[S:18]1[CH:19]=[CH:20][C:16]([CH2:7][CH2:8][CH2:9][C:10]([OH:12])=[O:11])=[CH:17]1

参与物

7

反应物 5

HCID 313海萝胶HCID 5234Halite (NaCl)HCID 14797氢氧化钾HCID 24654水合肼HCID 6611424[2-Oxo-2-(3-thienyl)ethyl]malonic acid

产物 1

HCID 110411434-(噻吩-3-基)丁酸收率 87.6%

试剂、催化剂与溶剂 1

HCID 1742,2’-[(1-甲基亚乙基)二(4,1-亚苯基氧亚甲基)]二环氧乙烷与α-氢-ω-羟基聚(氧-1,2-亚乙基)的聚合物溶剂

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.

后处理

  1. temperatureThis solution was heated
  2. temperatureat reflux for 6 hours
  3. customthe crude reaction mixture
  4. extractionextracted with ether (3×70 mL)
  5. dry with materialThe combined organic extracts were dried over Na2SO4
  6. concentrationconcentrated, in vacuo

来源与证据

ORD记录
ord-d7d51544825c4bb7a548bd1885f197b6
来源数据集
uspto-grants-1998_03
专利号
US05726312

关联笔记

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