Water → HCID 53415539, 화합물

HRID 271113노트

반응식

HRID 271113 반응식
[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

참가 물질

7

반응물 5

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

생성물 1

HCID 53415539HCID 53415539, 화합물수율 75%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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)+.

후처리

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

출처 및 근거

ORD 기록
ord-d22a83343bec4204b1b002ed6c4b7e53
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07452885B2

반응 노트

불러오는 중…