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Ammonia → 5-Aminomethyl-1-(3-dimethylamino-propyl)-1-(4-fluoro-phenyl)-1,3-dihydro-isobenzofuran

HRID 432043
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HRID 432043 반응식
[CH3:1][N:2]([CH3:25])[CH2:3][CH2:4][CH2:5][C:6]1([C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)[C:14]2[C:9](=[CH:10][C:11]([C:15]#[N:16])=[CH:12][CH:13]=2)[C:8](=O)[O:7]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].S(=O)(=O)(O)O.N>C1COCC1.CCOCC.C1(C)C=CC=CC=1.O>[NH2:16][CH2:15][C:11]1[CH:10]=[C:9]2[C:14](=[CH:13][CH:12]=1)[C:6]([CH2:5][CH2:4][CH2:3][N:2]([CH3:25])[CH3:1])([C:18]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=1)[O:7][CH2:8]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 222AmmoniaHCID 1118Sulfuric AcidHCID 114845261-(3-(Dimethylamino)propyl)-1-(4-fluorophenyl)-1,3-dihydro-3-oxo-5-isobenzofurancarbonitrileHCID 21226445Aluminium lithium hydride

생성물 1

HCID 114729275-Aminomethyl-1-(3-dimethylamino-propyl)-1-(4-fluoro-phenyl)-1,3-dihydro-isobenzofuran수율 84%

시약·촉매·용매 4

HCID 962Water용매
HCID 1140Toluene용매
HCID 3283Diethyl Ether용매2회
HCID 8028Tetrahydrofuran용매

실험 절차

1-(3-Dimethylamino-propyl)-1-(4-fluoro-phenyl)-3-oxo-1,3-dihydro-isobenzofuran-5-carbonitrile (5.4 g, 16.2 mmol) was dissolved in dry THF (5 mL) and diluted with dry ether (50 mL). This solution was added dropwise to a refluxing suspension of lithium aluminium hydride (2.5 g, 65 mmol) in dry ether (150 mL) over 10-15 minutes, after which the resulting suspension was heated at reflux for a further 4 h. The solution was allowed to cool to room temperature and was stirred at room temperature overnight. The reaction was quenched with a minimum of water, and the resulting solution/suspension was dried over anhydrous magnesium sulfate. The mixture was filtered, and the solid cake was washed with THF. The combined filtrates were evaporated to give an oil. The oil was dissolved in toluene (200 mL) and was stirred with an aqueous solution of sulfuric acid (10 ml, 70% v/v) for 3 h. The mixture was diluted with water, and the pH was adjusted to >9 by the addition of aqueous ammonia solution (25% w/v). The toluene was separated, and the aqueous phase was extracted with further toluene. The combined toluene extracts were dried over anhydrous magnesium sulfate, filtered and evaporated to give the title compound as a yellow oil (4.4 g, 84%). 1H NMR (CDCl3): δ 1.25-1.40 (m, 1H), 1.40-1.55 (m, 1H), 2.11 (ddd, 1H), 2.13 (t, 3H), 2.15 (ddd, 1H), 2.21 (t, 2H), 3.85 (s, 2H), 5.11 (d, 1H), 5.14 (d, 1H), 6.96 (t, 2H), 7.15 (s, 1H), 7.21 (d, 1H), 7.22 (d, 1H), 7.45 (dd, 2H).

후처리

  1. temperatureafter which the resulting suspension was heated
  2. temperatureat reflux for a further 4 h
  3. customThe reaction was quenched with a minimum of water
  4. dry with materialthe resulting solution/suspension was dried over anhydrous magnesium sulfate
  5. filtrationThe mixture was filtered
  6. washthe solid cake was washed with THF
  7. customThe combined filtrates were evaporated
  8. customto give an oil
  9. customThe toluene was separated
  10. extractionthe aqueous phase was extracted with further toluene
  11. dry with materialThe combined toluene extracts were dried over anhydrous magnesium sulfate
  12. filtrationfiltered
  13. customevaporated

출처 및 근거

ORD 기록
ord-41ffbe9cb9e54d38b47df74f46354aec
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06660873B2

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