Hydrazine hydrate (1:1) → HCID 59309723, Verbindung

HRID 1512988Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1512988
[Cl:1][C:2]1[C:3]([N:11]2C(=O)C3C(=CC=CC=3)C2=O)=[CH:4][C:5]([SH:10])=[C:6]([O:8][CH3:9])[CH:7]=1.O.NN>O1CCCC1>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([SH:10])=[CH:4][C:3]=1[NH2:11]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 59310058HCID 59310058, Verbindung

Produkt 1

HCID 59309723HCID 59309723, VerbindungAusbeute 77,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 5-chloro-4-(1,3-dioxo-1,3-dihydroisoindol-2-yl)-2-mercaptoanisole (0.65 g) in tetrahydrofuran (20 mL) was added hydrazine monohydrate (0.5 mL), and the mixture was heated at reflux for 1.5 hours. The insoluble material was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1) to give the title compound (0.3 g).

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 1.5 hours
  3. customThe insoluble material was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (eluent: n-hexane−n-hexane/ethyl acetate=1/1)

Quellen und Nachweise

ORD-Eintrag
ord-2b7a1a65ef164af5b1452f02e381f2e5
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08217069B2

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