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Diisopropylamine → (2R)-1-[2-(5-bromo-1-benzofuran-2-yl)ethyl]-2-methylpyrrolidine

HRID 2416137
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HRID 2416137 반응식
[C:1]([CH:4]([CH:6]([C:8](O)=O)O)O)(O)=O.[CH3:11][C@@H:12]1[CH2:16][CH2:15][CH2:14][NH:13]1.C(=O)([O-])[O-].[K+].[K+].CC1C=CC(S(OCCC#C)(=O)=O)=CC=1.[Br:38][C:39]1[CH:44]=[CH:43][C:42]([OH:45])=[C:41](I)[CH:40]=1.C(NC(C)C)(C)C>C(#N)C.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.[Cu](I)I>[Br:38][C:39]1[CH:44]=[CH:43][C:42]2[O:45][C:4]([CH2:6][CH2:8][N:13]3[CH2:14][CH2:15][CH2:16][C@H:12]3[CH3:11])=[CH:1][C:41]=2[CH:40]=1
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참가 물질

9

반응물 5

HCID 7912DiisopropylamineHCID 11430Potassium CarbonateHCID 2720203-Butynyl p-toluenesulfonateHCID 109245324-Bromo-2-iodophenolHCID 23404464(2R)-2-Methylpyrrolidine tartrate

생성물 1

HCID 11220543(2R)-1-[2-(5-bromo-1-benzofuran-2-yl)ethyl]-2-methylpyrrolidine

시약·촉매·용매

3
HCID 83717Copper iodide촉매HCID 178418476HCID 178418476, 화합물촉매HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

(2R)-2-Methylpyrrolidine tartrate (1.17 g, 5.0 mmol), and potassium carbonate (1.38 g, 10.0 mmol) were combined in acetonitrile (20 mL) and heated at 60° C. for 1 hour. The mixture was treated with 3-butynyl 4-methylbenzenesulfonate (673 mg, 3.0 mmol) and heated at about 60° C. overnight. The mixture was cooled to about 5° C. and filtered. The mixture was treated with the product from Example 3A (300 mg, 1.0 mmol), diisopropylamine (1.20 g, 11.8 mmol), dichlorobis(triphenylphosphine)palladium (II) (35.1 mg, 0.05 mmol), and copper iodide (38.0 mg, 0.20 mmol). After stirring overnight at about 30° C., the mixture was concentrated to dryness. The residue in ethyl acetate (20 mL) was washed with 5% NaHCO3 (20 mL×2) and 25% brine (25 mL). The organic phase was separated, dried over anhydrous Na2SO4, filtered, and the filtrate concentrated to dryness to provide the title compound. MS (esi): 308, 310 (M+H)+; 1H-NMR (CDCl3) δ 7.58 (1H, d, J=1.7 Hz), 7.27 (2H, m), 6.38 (1H, s), 3.20 (2H, m), 2.95 (2H, m), 2.43 (1H, m), 2.28 (1H, m), 2.19 (1H, q, J=8.8 Hz), 1.95 (1H, m), 1.75 (2H, m), 1.42 (1H, m), 1.13 (3H, d, J=6.2 Hz); 13C-NMR (CDCl3) δ 158.8, 152.9,130.6, 125.7, 122.6, 115.2,111.9, 101.8, 60.0, 53.9, 51.9, 32.9, 28.4, 22.0, 19.3.

후처리

  1. temperatureheated at about 60° C. overnight
  2. temperatureThe mixture was cooled to about 5° C.
  3. filtrationfiltered
  4. concentrationthe mixture was concentrated to dryness
  5. washThe residue in ethyl acetate (20 mL) was washed with 5% NaHCO3 (20 mL×2) and 25% brine (25 mL)
  6. customThe organic phase was separated
  7. dry with materialdried over anhydrous Na2SO4
  8. filtrationfiltered
  9. concentrationthe filtrate concentrated to dryness

출처 및 근거

ORD 기록
ord-4719ed18c1af4091abfc23a7f991e5a7
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06822101B2

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