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Hydrochloric Acid → HCID 69931466, 화합물

HRID 429448
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HRID 429448 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([O:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[C:26]3[C:21](=[CH:22][CH:23]=[C:24]([O:27][CH3:28])[CH:25]=3)[O:20][C:19](=O)[C:18]=2[C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)=[CH:13][CH:12]=1)(=O)[CH3:8].Cl.C(=O)([O-])[O-].[K+].[K+].Cl.ClCC[N:47]1[CH2:51][CH2:50][CH2:49][CH2:48]1.[I-].[Na+]>O1CCCC1.O.C(O)C.[Pd]>[CH3:28][O:27][C:24]1[CH:25]=[C:26]2[C:21](=[CH:22][CH:23]=1)[O:20][CH2:19][C@@H:18]([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C@H:17]2[C:14]1[CH:13]=[CH:12][C:11]([O:10][CH2:7][CH2:8][N:47]2[CH2:51][CH2:50][CH2:49][CH2:48]2)=[CH:16][CH:15]=1
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참가 물질

11

반응물 6

HCID 313Hydrochloric AcidHCID 5238Sodium IodideHCID 11430Potassium CarbonateHCID 816681-(2-Chloroethyl)pyrrolidine hydrochlorideHCID 18355594HCID 18355594, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 69931466
HCID 69931466, 화합물

시약·촉매·용매 4

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
65 °C

실험 절차

Lithium aluminium hydride (0.96 g, 2.54 mmol) was added in small portions to a stirred solution of 4-(4-acetoxyphenyl)-3-phenyl-6-methoxy-coumarin (0.49 g, 1.27 mmol) in tetrahydrofuran (75 ml). The resulting mixture was stirred for 30 min., 6M hydrochloric acid (4 ml) added dropwise, and the mixture heated to 65° C. for 3 h. The mixture was cooled to room temperature, diluted with 100 ml water, and the product extracted into ethyl acetate (2×100 ml). The extracts were washed with brine, dried over sodium sulfate and evaporated to give a yellow gum. This gum was dissolved in ethanol (100 ml), and palladium on carbon (5%, 0.045 g, 0.02 mmol) added, then the mixture was hydrogenated for 18 h. The catalyst was removed by filtration and the solvents evaporated to give an orange gum, which was vacuum dried. The gum was dissolved in dry acetone (20 ml) then potassium carbonate (1.87 g, 13.50 mmol), 1-(2-chloroethyl)pyrrolidine hydrochloride (0.257 g, 1.51 mmol) and sodium iodide (0.01 g, catalyst) were added and the mixture heated to 60° C. for 20 h. The inorganic solids were removed by filtration and the solvent removed to give an orange gum, which was purified by column chromatography on silica gel 60 with 9:1 dichloromethane/methanol eluent. This gave the product as a pale orange gum, which was vacuum dried.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. extractionthe product extracted into ethyl acetate (2×100 ml)
  3. washThe extracts were washed with brine
  4. dry with materialdried over sodium sulfate
  5. customevaporated
  6. customto give a yellow gum
  7. waitthe mixture was hydrogenated for 18 h
  8. customThe catalyst was removed by filtration
  9. customthe solvents evaporated
  10. customto give an orange gum, which
  11. customdried
  12. dissolutionThe gum was dissolved in dry acetone (20 ml)
  13. temperaturethe mixture heated to 60° C. for 20 h
  14. customThe inorganic solids were removed by filtration
  15. customthe solvent removed
  16. customto give an orange gum, which
  17. customwas purified by column chromatography on silica gel 60 with 9:1 dichloromethane/methanol eluent

출처 및 근거

ORD 기록
ord-fb74769504b0444e909a96a1bd9da23a
출처 데이터셋
uspto-grants-2001_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06316494B1

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