Water → HCID 53415539、化合物

HRID 271113ノート

反応式

HRID 271113 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)[CH:5]=[CH:6][CH:7]=1.C([O-])(O)=[O:17].[Na+].[O-]S([O-])(=O)=O.[Mg+2].[Mn]([O-])(=O)(=O)=O.[K+].[OH2:33]>CC(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([C:8](=[O:17])[C:9]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[O:33])[CH:5]=[CH:6][CH:7]=1

参加物

7

反応物 5

HCID 962WaterHCID 24083Sulfuric acid magnesium salt (1:1)HCID 516875Potassium PermanganateHCID 516892Sodium BicarbonateHCID 598345694-[(3-Bromophenyl)ethynyl]pyridine

生成物 1

HCID 53415539HCID 53415539、化合物収率 75%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 4-[(3-bromophenyl)ethynyl]pyridine (1.81 g, 7.0 mmol) in acetone (63 mL) is added a warm (˜40° C.) solution of NaHCO3 (0.35 g, 4.20 mmol) and MgSO4 (1.26 g, 10.50 mmol) in H2O (63 mL) followed by the addition of solid potassium permanganate (2.43 g, 15.40 mmol) in one portion. After stirring at room temperature for 4 minutes, the reaction mixture is extracted with 1/1 Et2O/hexane. The extracts are combined, dried over MgSO4 and concentrated to dryness to afford the title compound (1.52 g, 75%) as a solid. Mp: 88-90° C. MS (+) ES: 289 (M+H)+.

後処理

  1. extractionthe reaction mixture is extracted with 1/1 Et2O/hexane
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-d22a83343bec4204b1b002ed6c4b7e53
出典データセット
uspto-grants-2008_11
特許番号
US07452885B2

反応ノート

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