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Sodium Iodide → Methyl 5-{[cyclohexyl(5-fluoro-3-methyl-1-benzofuran-2-yl)methyl]amino}pyridine-2-carboxylate

HRID 2091063
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HRID 2091063 반응식
[CH:1]1([CH:7]([C:9]2[O:10][C:11]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:12]=3[C:13]=2[CH3:14])O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.S(Cl)(Cl)=O.C(=O)([O-])O.[Na+].[NH2:29][C:30]1[CH:31]=[CH:32][C:33]([C:36]([O:38][CH3:39])=[O:37])=[N:34][CH:35]=1.[I-].[Na+].C(=O)([O-])[O-].[Na+].[Na+].[Cl-].[NH4+]>C1(C)C=CC=CC=1.CN(C)C=O>[CH:1]1([CH:7]([NH:29][C:30]2[CH:31]=[CH:32][C:33]([C:36]([O:38][CH3:39])=[O:37])=[N:34][CH:35]=2)[C:9]2[O:10][C:11]3[CH:18]=[CH:17][C:16]([F:19])=[CH:15][C:12]=3[C:13]=2[CH3:14])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
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참가 물질

10

반응물 7

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 24386Thionyl ChlorideHCID 25517Ammonium ChlorideHCID 516892Sodium BicarbonateHCID 12457877Methyl 5-aminopyridine-2-carboxylateHCID 66777937Cyclohexyl(5-fluoro-3-methyl-1-benzofuran-2-yl)methanol

생성물 1

HCID 66777793Methyl 5-{[cyclohexyl(5-fluoro-3-methyl-1-benzofuran-2-yl)methyl]amino}pyridine-2-carboxylate수율 40.1%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6228Dimethylformamide용매

실험 절차

To a solution (15 mL) of cyclohexyl(5-fluoro-3-methyl-1-benzofuran-2-yl)methanol (1.50 g) synthesized in Example A37(2) in toluene was added thionyl chloride (625 μL), and the mixture was stirred at room temperature for 3 hr. The reaction mixture was poured into ice-cooled saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure to give a brown oil. To a mixture of the obtained oil, methyl 5-aminopyridine-2-carboxylate (957 mg), sodium iodide (1.71 g) and N,N-dimethylformamide (15 mL) was added sodium carbonate (1.21 g), and the mixture was stirred at 80° C. overnight. Saturated aqueous ammonium chloride solution was added to quench the reaction, and the reaction mixture was extracted with ethyl acetate. The extract was washed with saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (10-50% ethyl acetate/hexane) to give the title object compound (909 mg, 40%) as a pale-brown solid.

후처리

  1. additionThe reaction mixture was poured into ice-
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customto give a brown oil
  7. stirringthe mixture was stirred at 80° C. overnight
  8. customto quench
  9. customthe reaction
  10. extractionthe reaction mixture was extracted with ethyl acetate
  11. washThe extract was washed with saturated brine
  12. dry with materialdried over magnesium sulfate
  13. concentrationconcentrated under reduced pressure
  14. customThe residue was purified by silica gel column chromatography (10-50% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-c1a73fd95d334af8b51e797ab3ef117d
출처 데이터셋
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08436043B2

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