1-Naphthyl Isothiocyanate → HCID 59857370, Verbindung

HRID 555401

Reaktionsgleichung

Reaktionsgleichung von HRID 555401
[C:1]([C:5]1[CH:18]=[CH:17][CH:16]=[CH:15][C:6]=1[O:7][C:8]1[C:13]([NH2:14])=[CH:12][CH:11]=[CH:10][N:9]=1)([CH3:4])([CH3:3])[CH3:2].[C:19]1([N:29]=[C:30]=[S:31])[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=[CH:21][CH:20]=1>O1CCOCC1>[C:1]([C:5]1[CH:18]=[CH:17][CH:16]=[CH:15][C:6]=1[O:7][C:8]1[C:13]([NH:14][C:30]([NH:29][C:19]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH:22]=[CH:21][CH:20]=2)=[S:31])=[CH:12][CH:11]=[CH:10][N:9]=1)([CH3:4])([CH3:2])[CH3:3]

Komponenten

4

Edukt 2

HCID 110801-Naphthyl Isothiocyanate2×HCID 286054272-(2-tert-Butylphenoxy)pyridin-3-amine

Produkt 1

HCID 59857370HCID 59857370, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A solution of 1b (40 mg, 0.17 mmol) and 1-naphtylisothiocyanate (34 mg, 0.18 mmol) in dioxane (2 mL) was heated at 60° C. for 6 h. More 1-naphtylisothiocyanate (34 mg, 0.18 mmol) was added and the mixture was heated at 60° C. for 8 days. The mixture was concentrated and the residue was purified by column chromatography on silica gel using a continuous gradient from 0% to 40% ethyl acetate in hexanes as eluent to afford 102a which was directly used in the next step. [M−H]−=426.18.

Aufarbeitung

  1. concentrationThe mixture was concentrated
  2. customthe residue was purified by column chromatography on silica gel using a continuous gradient from 0% to 40% ethyl acetate in hexanes as eluent

Quellen und Nachweise

ORD-Eintrag
ord-ff6f066617144174b7fa06cc4e5ab556
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08053450B2

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