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Hydrochloric Acid → HCID 17906331, 화합물

HRID 852104
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HRID 852104 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.Br[CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][C:21]([C:24]2[C:28]3[CH:29]=[CH:30][C:31]([F:33])=[CH:32][C:27]=3[O:26][N:25]=2)=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].[ClH:42]>O.C(Cl)(Cl)Cl.CCOCC.C(#N)C>[ClH:42].[F:33][C:31]1[CH:30]=[CH:29][C:28]2[C:24]([C:21]3[CH:20]=[CH:19][C:18]([O:17][CH2:16][CH2:15][N:11]4[CH2:10][CH2:9][CH:8]([C:5]5[CH:6]=[CH:7][C:2]([F:1])=[CH:3][CH:4]=5)[CH2:13][CH2:12]4)=[CH:23][CH:22]=3)=[N:25][O:26][C:27]=2[CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

10

반응물 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 27591364-(4-Fluorophenyl)piperidineHCID 17906318HCID 17906318, 화합물

생성물 1

HCID 17906331HCID 17906331, 화합물수율 48%

시약·촉매·용매 4

HCID 962
Water
용매
HCID 3283Diethyl Ether용매
HCID 6212Chloroform용매
HCID 6342Acetonitrile용매

실험 절차

Add 4-(4-fluoro-phenyl)-piperidine (133 mg, 0.744 mol) (See Table No.1, SM 2) to a suspension of 3-[4-(2-bromo-ethoxy)-phenyl]-6-fluoro-benzo[d]isoxazole (250 mg, 0.744 mol) in a mixture of water:acetonitrile (0.1 mL:2.5 mL). Then add potassium carbonate (164 mg, 1.63 mmol) and potassium iodide (12 mg, 1.07 mmol) and heat at reflux for 8 hours. Stir at room temperature for 72 hours, filter the suspension and wash the solid thoroughly with dichloromethane. Dilute the resulting solution with dichloromethane (5 mL) and wash with water (5 mL), 10% HCl (5 mL), water (5 mL), saturated sodium chloride (5 mL), dry (MgSO4), filter and evaporate to give a white solid. Dissolve the solid in a minimum amount of chloroform and add 1.0 M HCl in ether and stir under a nitrogen atmosphere for 1 hour. Collect the solid by vacuum filtration, wash thoroughly with ether and dry to give the title compound (168 mg, 48% Yield). Microanalysis (C, H, N) is consistent with the final, desired compound. mp-235-239° C.

후처리

  1. temperatureat reflux for 8 hours
  2. filtrationfilter the suspension
  3. washwash the solid thoroughly with dichloromethane
  4. additionDilute the resulting solution with dichloromethane (5 mL)
  5. washwash with water (5 mL), 10% HCl (5 mL), water (5 mL), saturated sodium chloride (5 mL)
  6. dry with materialdry (MgSO4)
  7. filtrationfilter
  8. customevaporate
  9. customto give a white solid
  10. stirringstir under a nitrogen atmosphere for 1 hour
  11. customCollect the solid
  12. filtrationby vacuum filtration
  13. washwash thoroughly with ether
  14. customdry

출처 및 근거

ORD 기록
ord-9dcd964128d34be3abefa55e5793302d
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07253165B2

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