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

HRID 535665

반응식

HRID 535665 반응식
[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

참가 물질

4

반응물 2

HCID 313Hydrochloric Acid2회HCID 59636709Diethyl 2-(6-methoxypyridin-2-yl)malonate

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
65 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-84a06a4b777748848d4e1887319362c8
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08859534B2

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