Water → HCID 67401690、化合物

HRID 909256ノート

反応式

HRID 909256 の反応式
[C:1]1([CH:7]2[NH:12][CH2:11][CH2:10][N:9]3[CH:13]=[CH:14][CH:15]=[C:8]23)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:16]([O:18][C:19](=[O:22])[CH2:20]Br)C.C(=O)([O-])[O-].[K+].[K+].O>C(#N)C.CC(=O)OCC>[CH3:16][O:18][C:19](=[O:22])[CH2:20][N:12]1[CH2:11][CH2:10][N:9]2[CH:13]=[CH:14][CH:15]=[C:8]2[CH:7]1[C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

7

反応物 4

HCID 962WaterHCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 27709101-phenyl-1H,2H,3H,4H-pyrrolo(1,2-a)pyrazine

生成物 1

HCID 67401690HCID 67401690、化合物収率 102.1%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of (1.0 g, 5.0 mmol) of 1-phenyl-1,2,3,4-tetrahydropyrrolo[1,2-a]pyrazine, 2-bromoacetic acid ethyl ester (587 μl, 5.3 mmol) and potassium carbonate (1.74 g, 12.6 mmol) in acetonitrile (20 ml) was heated for 2 h under reflux. Water (10 ml) and EA (20 ml) were then added, stirring was carried out for 15 min, and the phases were separated. The organic phase was dried over MgSO4, filtered and concentrated in vacuo. 1.38 g of 2-(1-phenyl-3,4-dihydropyrrolo[1,2-a]pyrazin-2(1H)-yl)acetic acid methyl ester were obtained as residue and used in the next step without further purification.

後処理

  1. temperaturewas heated for 2 h
  2. temperatureunder reflux
  3. customthe phases were separated
  4. dry with materialThe organic phase was dried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1f725b3d923f497e9d14be00706158a9
出典データセット
uspto-grants-2011_09
特許番号
US08017772B2

反応ノート

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