Methylamine Acetate → 4-(5-Chloroindol-3-yl)-2-methylamino-4-oxo-2-butenoic acid ethyl ester

HRID 2083873ノート

反応式

HRID 2083873 の反応式
[CH2:1]([O:3][C:4](=[O:20])[C:5](O)=[CH:6][C:7]([C:9]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([Cl:18])[CH:16]=2)[NH:11][CH:10]=1)=[O:8])[CH3:2].C(O)(=O)C.[CH3:25][NH2:26]>CCO>[CH2:1]([O:3][C:4](=[O:20])[C:5]([NH:26][CH3:25])=[CH:6][C:7]([C:9]1[C:17]2[C:12](=[CH:13][CH:14]=[C:15]([Cl:18])[CH:16]=2)[NH:11][CH:10]=1)=[O:8])[CH3:2]

参加物

4

反応物 2

HCID 13000541Methylamine AcetateHCID 178473094HCID 178473094、化合物

生成物 1

HCID 600774434-(5-Chloroindol-3-yl)-2-methylamino-4-oxo-2-butenoic acid ethyl ester収率 38%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 0.59 g (2.0 mmol) of 4-(5chloroindol-3-yl)-2-hydroxy-4-oxo-2-butenoic acid ethyl ester prepared in Example 1(1) in 95% EtOH (10 ml) was added 0.55 g (6.0 mmol) of methylamine acetate. After refluxing for 2.5 hours, the reaction mixture was concentrated and the residue was dissolved in ethyl acetate. The ethyl acetate was washed with water, dried, and then concentrated. The resulting residue was chromatographed on silica gel (ethyl acetate as eluant) to give 0.23 g of the titled compound as oil. Yield: 38%.

後処理

  1. temperatureAfter refluxing for 2.5 hours
  2. concentrationthe reaction mixture was concentrated
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe ethyl acetate was washed with water
  5. customdried
  6. concentrationconcentrated
  7. customThe resulting residue was chromatographed on silica gel (ethyl acetate as eluant)

出典と根拠

ORDレコード
ord-34d02b7ece3c4f959ad3228977aeb796
出典データセット
uspto-grants-2004_04
特許番号
US06716605B2

反応ノート

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