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Methyl iodide → HCID 18969744, 화합물

HRID 399067
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HRID 399067 반응식
[CH3:1][N:2]([CH3:11])[C:3](=[O:10])[CH2:4][C:5]1[CH:9]=[CH:8][S:7][CH:6]=1.[Li+].[CH3:13]C([N-]C(C)C)C.CI>C1COCC1>[CH3:11][N:2]([CH3:1])[C:3](=[O:10])[CH:4]([C:5]1[CH:9]=[CH:8][S:7][CH:6]=1)[CH3:13]
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 2724682Lithium diisopropylamideHCID 23273495Thiophene,3-(N,N-diMe acetamido)

생성물 1

HCID 18969744HCID 18969744, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of acetamide from Step 1 (510 mg) in THF (15 mL) at -78° C. was added LDA (mono THF, 1.5M, cyclohexane, 250 μL) followed by MeI (700 μL) after 30 min. The mixture was warmed to r.t., quenched with a saturated NH4Cl sol. and then extracted with Et2O. The organic phase was washed with H2O, brine, dried (MgSO4) and the solvents evaporated. The residue was purified by flash chromatography (silica gel; hexane/EtOAc (60:40)) to afford the title compound as a oil.

후처리

  1. customquenched with a saturated NH4Cl sol.
  2. extractionextracted with Et2O
  3. washThe organic phase was washed with H2O, brine
  4. dry with materialdried (MgSO4)
  5. customthe solvents evaporated
  6. customThe residue was purified by flash chromatography (silica gel; hexane/EtOAc (60:40))

출처 및 근거

ORD 기록
ord-94db0e5ad56541c6b9bafec4d3fad021
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05817700

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