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Lithium Hydroxide → N-benzyl-2-ethynyl-4-methylthiazole-5-carboxamide

HRID 2381776
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HRID 2381776 반응식
[CH2:1]([NH:8][C:9]([C:11]1[S:15][C:14](Br)=[N:13][C:12]=1[CH3:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:18](N(CC)C(C)C)(C)[CH3:19].C[Si](C#C)(C)C.[OH-].[Li+]>C1(C)C=CC=CC=1.C(OCC)(=O)C.[Cu]I.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[CH2:1]([NH:8][C:9]([C:11]1[S:15][C:14]([C:18]#[CH:19])=[N:13][C:12]=1[CH3:17])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

9

반응물 4

HCID 3939Lithium HydroxideHCID 66111TrimethylsilylacetyleneHCID 81531DiisopropylethylamineHCID 579593962-Bromo-4-methyl-thiazole-5-carboxylic acid benzylamide

생성물 1

HCID 73213266N-benzyl-2-ethynyl-4-methylthiazole-5-carboxamide수율 93%

시약·촉매·용매 4

HCID 24350
Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 1140Toluene용매
HCID 8857Ethyl Acetate용매

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온도
35 °C

실험 절차

To a solution of N-benzyl-2-bromo-4-methylthiazole-5-carboxamide (0.10 g, 0.32 mmol) in anhydrous toluene (1 mL) was added copper(I) iodide (0.001 g, 0.006 mmol), dichlorobis(triphenylphosphine)palladium(II) (0.005 g, 0.006 mmol), and N,N-diisopropylethylamine (0.17 mL, 0.97 mmol). The reaction mixture was degassed and the reaction flask was filled with nitrogen followed by the addition of trimethylsilylacetylene (0.089 mL, 0.64 mmol). The reaction mixture was heated at 35° C. for 3 hours, cooled to ambient temperature and treated with 1 M aqueous lithium hydroxide (1.0 mL) for 5 minutes, diluted with ethyl acetate (10 mL), washed with water (3 mL) and brine (3 mL). The organic layer was dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (ethyl acetate:hexanes, 1:1) to afford the title compound as a brown solid (0.035 g, 93%): 1H NMR (300 MHz, CDCl3) δ 7.43-7.21 (m, 5H), 6.17 (t, J=5.7 Hz, 1H), 4.56 (d, J=5.7 Hz, 2H), 3.49 (s, 1H), 2.65 (s, 3H); MS (ES+) m/z 257.2 (M+1).

후처리

  1. customThe reaction mixture was degassed
  2. additionthe reaction flask was filled with nitrogen
  3. temperaturecooled to ambient temperature
  4. washwashed with water (3 mL) and brine (3 mL)
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by column chromatography (ethyl acetate:hexanes, 1:1)

출처 및 근거

ORD 기록
ord-4b963e15520f4d18af7f06ed71b2bad1
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08258160B2

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