Ethyl Acetoacetate → HCID 22387816, 화합물

HRID 1699797노트

반응식

HRID 1699797 반응식
[N+](C1C=C([N+]([O-])=O)C=CC=1O)([O-])=O.[NH2:14][N:15]1[CH:25]=[CH:24][C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:17][CH2:16]1.C(=O)([O-])[O-].[K+].[K+].[C:32]([O:38][CH2:39][CH3:40])(=[O:37])[CH2:33][C:34]([CH3:36])=O>C(O)C>[CH2:39]([O:38][C:32]([C:33]1[C:34]([CH3:36])=[N:14][N:15]2[CH:16]=[CH:17][C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:24][C:25]=12)=[O:37])[CH3:40]

참가 물질

5

반응물 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 22388182HCID 22388182, 화합물

생성물 1

HCID 22387816HCID 22387816, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Ethyl N-aminoisonicotinate 2,4-dinitrophenol salt (10.2 g) was suspended in ethanol (147 ml), and potassium carbonate (3.77 g) was added, which was followed by stirring at room temperature for 30 min. To the mixture was added ethyl acetoacetate (3.69 ml), and the mixture was stirred at 60° C. for 5 hr with heating. The insoluble matter was filtered off and the filtrate was concentrated to dryness under reduced pressure. The residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=7/1) to give the objective compound (2.70 g) as an amber-colored solid.

후처리

  1. stirringthe mixture was stirred at 60° C. for 5 hr
  2. temperaturewith heating
  3. filtrationThe insoluble matter was filtered off
  4. concentrationthe filtrate was concentrated to dryness under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (eluent: hexane/ethyl acetate=7/1)

출처 및 근거

ORD 기록
ord-34280b9e3728451d80768e166f217be5
출처 데이터셋
uspto-grants-2002_02
특허 번호
US06348474B1

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