Ethyl 7-amino-4-oxo-4H-chromene-2-carboxylate → Ethyl 7-Amino-2-chromancarboxylate

HRID 49459노트

반응식

HRID 49459 반응식
[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[CH:7]=[C:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[O:9]2)=[CH:4][CH:3]=1>C(O)C.Cl.[Pd]>[NH2:1][C:2]1[CH:11]=[C:10]2[C:5]([CH2:6][CH2:7][CH:8]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[O:9]2)=[CH:4][CH:3]=1

참가 물질

5

반응물 1

HCID 10728325Ethyl 7-amino-4-oxo-4H-chromene-2-carboxylate

생성물 1

HCID 10632774Ethyl 7-Amino-2-chromancarboxylate수율 89%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

A solution of ethyl 7-amino-4-oxo-4H-chromene-2-carboxylate (1.00 g, 4.3 mmol) in ethanol and concentrated HCl (5 mL) is hydrogenated over 10% Pd/C (0.5 g) at 50 psi for 72 h at ambient temperature. The reaction mixture is filtered and the filtrate is concentrated in vacuo. The resultant residue is dissolved in ethyl acetate and washed with saturated aqueous NaHCO3. The organic phase is dried over MgSO4, and concentrated in vacuo to afford the title compound as an amber oil, 0.85 g (89% yield), identified by NMR and mass spectral analyses.

후처리

  1. filtrationThe reaction mixture is filtered
  2. concentrationthe filtrate is concentrated in vacuo
  3. dissolutionThe resultant residue is dissolved in ethyl acetate
  4. washwashed with saturated aqueous NaHCO3
  5. dry with materialThe organic phase is dried over MgSO4
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e2da5b6fc92c4373bfb43f28abe30963
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706757B2

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