Hydrochloric Acid → Ethyl 2-(6-methoxypyridin-2-YL)acetate

HRID 535665

反応式

HRID 535665 の反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH:9](C(OCC)=O)[C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:5][CH:4]=1.Cl>C(O)C>[CH3:1][O:2][C:3]1[N:8]=[C:7]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])[CH:6]=[CH:5][CH:4]=1

参加物

4

反応物 2

HCID 313Hydrochloric Acid2 回HCID 59636709Diethyl 2-(6-methoxypyridin-2-yl)malonate

生成物 1

HCID 55263200Ethyl 2-(6-methoxypyridin-2-YL)acetate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

A solution of diethyl 2-(6-methoxypyridin-2-yl)malonate (1.0 g, 3.74 mmol) and hydrochloric acid (1 M) (20 mL, 20.0 mmol) in ethanol (10 mL) was heated at 65° C. overnight. The solvent was removed under reduced pressure. The residue was dissolved in ethanol (15 mL) and hydrochloric acid (conc.) (0.5 mL, 6.00 mmol) was added. The reaction mixture was heated at 65° C. for 4 h. The solvent was removed under reduced pressure. Ethyl acetate and saturated NaHCO3 aqueous solution were added. The organic layer was separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried (Na2SO4) and concentrated to give the product. Yield: 0.69 g (94%).

後処理

  1. customThe solvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in ethanol (15 mL)
  3. customThe solvent was removed under reduced pressure
  4. additionEthyl acetate and saturated NaHCO3 aqueous solution were added
  5. customThe organic layer was separated
  6. extractionthe aqueous layer was extracted with ethyl acetate
  7. dry with materialThe combined organic layers were dried (Na2SO4)
  8. concentrationconcentrated
  9. customto give the product

出典と根拠

ORDレコード
ord-84a06a4b777748848d4e1887319362c8
出典データセット
uspto-grants-2014_10
特許番号
US08859534B2

関連ノート

読み込み中…