Cesium carbonate → HCID 68992282, Verbindung

HRID 69462Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 69462
[O:1]1[C:5]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:25][CH2:24][C:23]5[C:18](=[CH:19][CH:20]=[C:21]([OH:26])[CH:22]=5)[C:17]4=[O:27])=[CH:12][C:11]=3[F:28])[CH2:6]2)[O:4][CH2:3][CH2:2]1.CS([CH2:33][C@@H:34]1[CH2:38][CH2:37][CH2:36][O:35]1)(=O)=O.C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C=O)C.C(OCC)(=O)C.O>[O:4]1[C:5]2([CH2:9][CH2:8][N:7]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[CH2:25][CH2:24][C:23]5[C:18](=[CH:19][CH:20]=[C:21]([O:26][CH2:33][C@@H:34]6[CH2:38][CH2:37][CH2:36][O:35]6)[CH:22]=5)[C:17]4=[O:27])=[CH:12][C:11]=3[F:28])[CH2:6]2)[O:1][CH2:2][CH2:3]1

Komponenten

7

Edukt 3

HCID 10796Cesium carbonateHCID 689879432-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-oneHCID 68988132(S)-2-methanesulfonylmethyl-tetrahydrofuran

Produkt 1

HCID 68992282HCID 68992282, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

A mixture of 2-[4-(1,4-dioxa-7-aza-spiro[4.4]non-7-yl)-3-fluorophenyl]-6-hydroxy-3,4-dihydro-2H-isoquinolin-1-one (6.9 g), (S)-2-methanesulfonylmethyl-tetrahydrofuran (3.9 g) and cesium carbonate (17.6 g) in DMF (81.6 mL) was heated overnight at 75° C. Then the reaction mixture was diluted with ethyl acetate and water. The organic phase was washed several times with water, dried over sodium sulfate and the solvent was removed in vacuum. In this way the product was obtained with molecular weight 468.53 (C26H29FN2O5); MS (ESI): 469 (M+H+).

Aufarbeitung

  1. washThe organic phase was washed several times with water
  2. dry with materialdried over sodium sulfate
  3. customthe solvent was removed in vacuum
  4. customIn this way the product was obtained with molecular weight 468.53 (C26H29FN2O5)

Quellen und Nachweise

ORD-Eintrag
ord-44f8eafca076464e8a27cb328f1a524d
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822495B2

Notizen zur Reaktion

Wird geladen…