HCID 86685931, Verbindung → HCID 71743949, Verbindung

HRID 2277603Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2277603
[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[N:6](CC1C=CC(OC)=CC=1)[C:5]2([CH3:22])[CH3:21]>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[C:7](=[O:11])[NH:6][C:5]2([CH3:22])[CH3:21]

Komponenten

3

Edukt 1

HCID 86685931HCID 86685931, Verbindung

Produkt 1

HCID 71743949HCID 71743949, VerbindungAusbeute 85,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

A solution of 5-chloro-2-(4-methoxy-benzyl)-3,3-dimethyl-2,3-dihydro-isoindol-1-one (0.38 g, 1.2 mmol) in trifluoro acetic acid (5 mL) was heated to reflux for 20 hours. After removal of trifluoro acetic acid under reduced pressure, the crude product was purified by flash column chromatography (silica gel 14 g, 5% to 50% ethyl acetate in DCM) to give the title compound (0.20 g, 85%) as a white solid. MS: 196.1 (M+H+).

Aufarbeitung

  1. temperatureto reflux for 20 hours
  2. customAfter removal of trifluoro acetic acid under reduced pressure
  3. customthe crude product was purified by flash column chromatography (silica gel 14 g, 5% to 50% ethyl acetate in DCM)

Quellen und Nachweise

ORD-Eintrag
ord-2419ad2b92e6414dad2c21b4e5ecc319
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09133158B2

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