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Sodium Methoxide → HCID 57744887, 화합물

HRID 1661493
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HRID 1661493 반응식
BrC1SC([C:7]([O:9][CH3:10])=[O:8])=C(NC)C=1C.[CH3:14][O-].[Na+].[Br:17][C:18]1[S:22][C:21]([C:23]([O:25]C)=O)=[C:20]([N:27]([CH3:34])[C:28](=[O:33])[C:29](F)(F)F)[C:19]=1[CH3:35]>CO>[Br:17][C:18]1[S:22][C:21]2[C:23]([OH:25])=[C:29]([C:7]([O:9][CH2:10][CH3:14])=[O:8])[C:28](=[O:33])[N:27]([CH3:34])[C:20]=2[C:19]=1[CH3:35]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10942334Sodium MethoxideHCID 66743799HCID 66743799, 화합물HCID 86631544HCID 86631544, 화합물

생성물 1

HCID 57744887HCID 57744887, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl 5-bromo-4-methyl-3-(methylamino)thiophene-2-carboxylate. Sodium methanolate (3.9 mL, 1.9 mmol) was added to a suspension of methyl 5-bromo-4-methyl-3-(2,2,2-trifluoro-N-methylacetamido)thiophene-2-carboxylate (0.70 g, 1.9 mmol) in MeOH (5 mL) and stirred for 1 hour. The solvent was removed, and the residue was dissolved in CHCl3, washed with water, brine, dried over MgSO4, and evaporated. The residue was purified by flash chromatography using EtOAc/hexanes to give the title compound. MS (ESI) m/z: Calculated 264.1; Observed; 265.9. 1H NMR (300 MHz, CDCl3) δ ppm 6.85 (1H, br. s.), 3.79 (3H, s), 3.06 (3H, s), 2.28 (3H, s).

후처리

  1. customThe solvent was removed
  2. dissolutionthe residue was dissolved in CHCl3
  3. washwashed with water, brine
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-f904d624e6b74f14901d0168ef73dd23
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030346B2

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