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Triethylamine → 3-(3-(3-Fluoro-4-(pyridin-2-ylmethoxy)-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine

HRID 1891863
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HRID 1891863 반응식
[F:1][C:2]1[CH:15]=[C:14]([CH2:16][CH2:17][N+:18]([O-:20])=O)[CH:13]=[CH:12][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1.C[O-].[Li+].C(=O)(O)[O-].[Na+].[C:29]([C:31]1[C:32]([NH2:38])=[N:33][C:34]([NH2:37])=[CH:35][CH:36]=1)#[CH:30].C(N(CC)CC)C>[Ti](Cl)(Cl)(Cl)Cl.O.O1CCCC1.C(OCC)(=O)C.CO>[F:1][C:2]1[CH:15]=[C:14]([CH:13]=[CH:12][C:3]=1[O:4][CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1)[CH2:16][C:17]1[CH:30]=[C:29]([C:31]2[C:32]([NH2:38])=[N:33][C:34]([NH2:37])=[CH:35][CH:36]=2)[O:20][N:18]=1
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참가 물질

11

반응물 5

HCID 8471TriethylamineHCID 516892Sodium BicarbonateHCID 4177230Lithium methanolateHCID 552816763-Ethynylpyridine-2,6-diamineHCID 592550802-(2-Fluoro4-(2-nitro-ethyl)-phenoxymethyl)pyridine

생성물 1

HCID 592550683-(3-(3-Fluoro-4-(pyridin-2-ylmethoxy)-benzyl)-isoxazol-5-yl)-pyridin-2,6-diamine
수율 39.7%

시약·촉매·용매 5

HCID 24193Titanium Tetrachloride촉매HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a methanol (20.0 mL) solution of 2-(2-fluoro-4-(2-nitro-ethyl)-phenoxymethyl)-pyridine (500 mg, 1.81 mmol) described in Manufacturing Example 87-1-3 was added lithium methoxide (137 mg, 3.61 mmol) under nitrogen atmosphere, which was stirred for 30 minutes at room temperature. The reaction mixture was concentrated under a reduced pressure, and dichloromethane (15.0 mL) and anhydrous tetrahydrofuran (7.00 mL) were added to the residue. Titanium (IV) chloride (656 μL, 5.97 mmol) was added dropwise to the reaction mixture on a dry ice-ethanol bath (−78° C.), and which was stirred for 30 minutes at room temperature. Aqueous sodium bicarbonate and ethyl acetate were added to the reaction mixture on an ice bath (0° C.), which was filtered through a Celite pad. The organic layer of the filtrate was extracted with ethyl acetate, and this organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain a crude product (300 mg). To a tetrahydrofuran (5.00 mL) solution of this crude product (150 mg) and 3ethynyl-pyridin-2,6-diamine (30.0 mg, 0.225 mmol) described in Manufacturing Example 13-1-3 was added triethylamine (94.1 μL, 0.675 mmol) at room temperature, which was stirred for 1 hour at room temperature. Water was added to the reaction solution, which was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate, and the solvent was evaporated under a reduced pressure. The residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:1→10:1) to obtain the title compound (35.0 mg, 39.7%).

후처리

  1. concentrationThe reaction mixture was concentrated under a reduced pressure, and dichloromethane (15.0 mL) and anhydrous tetrahydrofuran (7.00 mL)
  2. additionwere added to the residue
  3. stirringwas stirred for 30 minutes at room temperature
  4. filtrationwas filtered through a Celite pad
  5. extractionThe organic layer of the filtrate was extracted with ethyl acetate
  6. washthis organic layer was washed with water and saturated aqueous sodium chloride
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationThe filtrate was concentrated under a reduced pressure
  10. customto obtain a crude product (300 mg)
  11. stirringwhich was stirred for 1 hour at room temperature
  12. extractionwas extracted with ethyl acetate
  13. washThe organic layer was washed with saturated aqueous sodium chloride
  14. dry with materialdried over anhydrous magnesium sulfate
  15. customthe solvent was evaporated under a reduced pressure
  16. customThe residue was purified by NH silica gel column chromatography (ethyl acetate:heptane=2:1→10:1)

출처 및 근거

ORD 기록
ord-1533a2368a5444a0bfa371791830a7ab
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08507530B2

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