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Sulfuric Acid → 7-Methoxy-3-(3-phenyl-4-(trifluoromethyl)isoxazol-5-yl)-4,5-dihydronaphtho[1,2-c]isoxazole

HRID 1506332
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HRID 1506332 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[N:13][OH:14])[CH2:8][CH2:7][CH2:6]2.C([Li])CCC.[C:20]1([C:26]2[C:30]([C:31]([F:34])([F:33])[F:32])=[C:29]([C:35](OC)=O)[O:28][N:27]=2)[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.S(=O)(=O)(O)O>C1COCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]1=[N:13][O:14][C:35]([C:29]3[O:28][N:27]=[C:26]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:30]=3[C:31]([F:34])([F:32])[F:33])=[C:8]1[CH2:7][CH2:6]2
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참가 물질

6

반응물 4

HCID 1118Sulfuric AcidHCID 52161626-Methoxy-1-tetralone oxime2회HCID 13508376Methyl 3-phenyl-4-(trifluoromethyl)isoxazole-5-carboxylate2회HCID 178418339Butyllithium

생성물 1

HCID 671703377-Methoxy-3-(3-phenyl-4-(trifluoromethyl)isoxazol-5-yl)-4,5-dihydronaphtho[1,2-c]isoxazole수율 26.6%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To 6-methoxy-3,4-dihydronaphthalen-1(2H)-one oxime (Intermediate 2, 0.328 g, 1.715 mmol) in 3 mL of THF, cooled to 0° C. was added butyllithium (1.372 mL, 3.43 mmol) dropwise over a period of 3 min. The contents were stirred at 0° C. for 30 min. A solution of methyl 3-phenyl-4-(trifluoromethyl)isoxazole-5-carboxylate (Intermediate 3, 0.31 g, 1.14 mmol) dissolved in 2 mL of THF was added over a period of 3 min. The pale yellow reaction mixture was allowed to come to room temperature and stirred for 20 min. To the reaction mixture was added 0.5 mL of conc. sulfuric acid dropwise over a period of 3 min. at 0° C. and the contents were allowed to come to room temperature over a period of 10 min., then stirred at room temperature for 1.5 h. The reaction mixture was concentrated under reduced pressure. Dioxane (5 mL) was added and the contents were heated at 100° C. for 1.5 h, and at room temperature for 18 h. The reaction mixture was concentrated under reduced pressure and partitioned between ethyl acetate (25 mL) and water (10 mL). The ethyl acetate layer was washed with sat. aq. sodium bicarbonate (15 mL), dried over sodium sulfate, concentrated and purified by silica gel column chromatography using hexane/ethyl acetate to yield 7-methoxy-3-(3-phenyl-4-(trifluoromethyl)isoxazol-5-yl)-4,5-dihydronaphtho[1,2-c]isoxazole (0.125 g, 0.303 mmol, 26.5% yield) as pale yellow solid. LC/MS M+1=413.0.

후처리

  1. additionwas added over a period of 3 min
  2. customto come to room temperature
  3. stirringstirred for 20 min
  4. waitto come to room temperature over a period of 10 min.
  5. stirringstirred at room temperature for 1.5 h
  6. concentrationThe reaction mixture was concentrated under reduced pressure
  7. additionDioxane (5 mL) was added
  8. temperaturethe contents were heated at 100° C. for 1.5 h
  9. waitat room temperature for 18 h
  10. concentrationThe reaction mixture was concentrated under reduced pressure
  11. custompartitioned between ethyl acetate (25 mL) and water (10 mL)
  12. washThe ethyl acetate layer was washed with sat. aq. sodium bicarbonate (15 mL)
  13. dry with materialdried over sodium sulfate
  14. concentrationconcentrated
  15. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-98aae930a1784e93854c51eac2cc052a
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216972B2

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