p-Toluenesulfonic acid → HCID 68988088, Verbindung

HRID 69419Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 69419
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12](=[O:16])[N:11]([C:17]1[CH:22]=[CH:21][C:20]([N:23]3[CH2:31][CH2:30][C:25]4(OCC[O:26]4)[CH2:24]3)=[CH:19][CH:18]=1)[CH2:10][CH2:9]2)[CH2:2][CH2:3][CH3:4].C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O>[CH2:1]([O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[C:12](=[O:16])[N:11]([C:17]1[CH:22]=[CH:21][C:20]([N:23]3[CH2:31][CH2:30][C:25](=[O:26])[CH2:24]3)=[CH:19][CH:18]=1)[CH2:10][CH2:9]2)[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 2

HCID 6101p-Toluenesulfonic acidHCID 689920606-butoxy-2-[4-(1,4-dioxa-7-azaspiro[4.4]non-7-yl)phenyl]-3,4-dihydro-2H-isoquinolin-1-one

Produkt 1

HCID 68988088HCID 68988088, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

A mixture of 6-butoxy-2-[4-(1,4-dioxa-7-azaspiro[4.4]non-7-yl)phenyl]-3,4-dihydro-2H-isoquinolin-1-one (1.40 g), p-toluenesulfonic acid (57 mg) and acetone (40 mL) was boiled under reflux for 12 hours and then concentrated. The residue was partitioned between sodium carbonate solution and ethyl acetate. The organic phase was dried and concentrated. The product with the molecular weight of 378.48 (C23H26N2O3) was obtained in this way; MS (ESI): 379 (M+H+).

Aufarbeitung

  1. temperatureunder reflux for 12 hours
  2. concentrationconcentrated
  3. customThe residue was partitioned between sodium carbonate solution and ethyl acetate
  4. customThe organic phase was dried
  5. concentrationconcentrated
  6. customThe product with the molecular weight of 378.48 (C23H26N2O3) was obtained in this way

Quellen und Nachweise

ORD-Eintrag
ord-6dfa129263f14983beed32c30c97c363
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08822495B2

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