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Cesium carbonate → HCID 89613655, Verbindung

HRID 1473336
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1473336
Br[C:2]1[CH:11]=[CH:10][CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][C:6]([S:12]([N:15](CC1C=CC(OC)=CC=1OC)[C:16]1[S:17][CH:18]=[CH:19][N:20]=1)(=[O:14])=[O:13])=[CH:7]2.CC1(C)C2C(=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=CC=2)OC2C(P(C3C=CC=CC=3)C3C=CC=CC=3)=CC=CC1=2.C(=O)([O-])[O-].[Cs+].[Cs+].[C:80]1([CH:86]2[CH2:90][CH2:89][CH2:88][NH:87]2)[CH:85]=[CH:84][CH:83]=[CH:82][CH:81]=1>C(Cl)Cl.C(O)(C(F)(F)F)=O.CO.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[C:80]1([CH:86]2[CH2:90][CH2:89][CH2:88][N:87]2[C:2]2[CH:11]=[CH:10][CH:9]=[C:8]3[C:3]=2[CH:4]=[CH:5][C:6]([S:12]([NH:15][C:16]2[S:17][CH:18]=[CH:19][N:20]=2)(=[O:13])=[O:14])=[CH:7]3)[CH:85]=[CH:84][CH:83]=[CH:82][CH:81]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 4

HCID 10796Cesium carbonateHCID 2618922-PhenylpyrrolidineHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 89613856HCID 89613856, Verbindung

Produkt 1

HCID 89613655HCID 89613655, VerbindungAusbeute 35 %

Reagenzien, Katalysatoren, Lösungsmittel 5

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 887MethanolLösungsmittelHCID 1140TolueneLösungsmittelHCID 6344DichloromethaneLösungsmittelHCID 6422Trifluoroacetic acidLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

A vial was charged with 5-bromo-N-(2,4-dimethoxybenzyl)-N-(thiazol-2-yl)naphthalene-2-sulfonamide (51.89 mg, 0.100 mmol), Xantphos (11.56 mg, 0.020 mmol), Pd2(dba)3 (9.15 mg, 9.99 μmol), and cesium carbonate (65.1 mg, 0.200 mmol). The vial was flushed with Ar (g), then toluene (999 μl) and 2-phenylpyrrolidine (19.12 μl, 0.130 mmol) were added in sequence. The vial was sealed and heated to 100° C. for 18 h. The mixture was partitioned between EtOAc and water. The layers were separated, and the organic extract was washed with brine. The combined aq. layers were extracted with EtOAc, and the organic layers were combined. The combined solution was dried over sodium sulfate, filtered, and concentrated. The residue was purified by chromatography on silica gel (0 to 50% EtOAc/Heptane) to give a clear oil. This oil was taken up in DCM (1 mL) and TFA (0.5 mL). After 2 h, the mixture was diluted with MeOH, then concentrated. The residue was taken up in diethyl ether, sonicated, then filtered. The collected solid was washed with diethyl ether (twice), dried under a stream of N2 (g) for 10 min, then dried under a high vacuum to give 5-(2-phenylpyrrolidin-1-yl)-N-(thiazol-2-yl)naphthalene-2-sulfonamide (15.25 mg, 0.035 mmol) as a white solid. 1H NMR (400 MHz, DMSO-d6) δ ppm=12.76 (br. s., 1H), 8.45 (d, J=9.0 Hz, 1H), 8.31 (d, J=1.7 Hz, 1H), 7.77 (dd, J=2.0, 8.9 Hz, 1H), 7.59 (d, J=8.1 Hz, 1H), 7.40 (d, J=7.1 Hz, 2H), 7.33 (t, J=7.9 Hz, 1H), 7.26 (d, J=4.6 Hz, 1H), 7.18 (t, J=7.5 Hz, 2H), 7.12-7.04 (m, 2H), 6.82 (d, J=4.6 Hz, 1H), 4.86-4.77 (m, 1H), 4.20-4.10 (m, 1H), 3.02 (dt, J=4.7, 8.9 Hz, 1H), 2.47-2.39 (m, 1H), 2.16-2.05 (m, 1H), 2.00-1.78 (m, 2H). m/z (ESI) 436.2 (M+H)+.

Aufarbeitung

  1. customThe vial was flushed with Ar (g)
  2. customThe vial was sealed
  3. customThe mixture was partitioned between EtOAc and water
  4. customThe layers were separated
  5. extractionthe organic extract
  6. washwas washed with brine
  7. extractionThe combined aq. layers were extracted with EtOAc
  8. dry with materialThe combined solution was dried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe residue was purified by chromatography on silica gel (0 to 50% EtOAc/Heptane)
  12. customto give a clear oil
  13. concentrationconcentrated
  14. customsonicated
  15. filtrationfiltered
  16. washThe collected solid was washed with diethyl ether (twice),
  17. dry with materialdried under a stream of N2 (g) for 10 min
  18. customdried under a high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-8af772cc83f74986aa65e7a4930e9433
Quelldatensatz
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09012443B2

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