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

HRID 2083873노트

반응식

HRID 2083873 반응식
[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]

참가 물질

4

반응물 2

HCID 13000541Methylamine AcetateHCID 178473094HCID 178473094, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%.

후처리

  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)

출처 및 근거

ORD 기록
ord-34d02b7ece3c4f959ad3228977aeb796
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06716605B2

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