Ethyl Acetoacetate → HCID 22387816、化合物

HRID 1072779ノート

反応式

HRID 1072779 の反応式
[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>[CH3:36][C:34]1[C:33]([C:32]([O:38][CH2:39][CH3:40])=[O:37])=[C:25]2[CH:24]=[C:18]([C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH:17]=[CH:16][N:15]2[N:14]=1

参加物

5

反応物 3

HCID 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 22388182HCID 22388182、化合物

生成物 1

HCID 22387816HCID 22387816、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-00ec18c89f014e61be3b942ae398d67b
出典データセット
uspto-grants-2005_06
特許番号
US06911469B2

反応ノート

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