HCID 13837186, Verbindung → HCID 18940705, Verbindung

HRID 355814

Reaktionsgleichung

Reaktionsgleichung von HRID 355814
[CH:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[C:3]([C:14](N2C=CN=C2)=O)[N:2]=1.[OH:21][NH:22][C:23](=[NH:26])[CH2:24][CH3:25]>C1(C)C=CC=CC=1.CN(C=O)C>[CH2:24]([C:23]1[N:26]=[C:14]([C:3]2[N:2]=[CH:1][C:13]3[NH:12][C:11]4[C:6]([C:5]=3[CH:4]=2)=[CH:7][CH:8]=[CH:9][CH:10]=4)[O:21][N:22]=1)[CH3:25]

Komponenten

5

Edukt 2

HCID 13837186HCID 13837186, VerbindungHCID 178458070HCID 178458070, Verbindung

Produkt 1

HCID 18940705HCID 18940705, VerbindungAusbeute 56,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of Compound 1 (1.05 g, 4 mmol) in a mixture of toluene (50 mL) and DMF (50 mL), N-hydroxypropanimidamide (0.53 g, 6 mmol) was added. The resulting mixture was heated at 140°-150° C. for 7 h, and stirring continued for 3 days at room temperture. The solvents were removed in vacuo, and the oily residue precipitated from water. The white solid (1.0 g) was dried and submitted to column chromatography on silica gel with CH2Cl2 /methanol(9:1) as eluent. This afforded the title compound (0.6 g, 56%). M.p. 146°-149° C.

Aufarbeitung

  1. additionwas added
  2. temperatureThe resulting mixture was heated at 140°-150° C. for 7 h
  3. customThe solvents were removed in vacuo
  4. customthe oily residue precipitated from water
  5. dry with materialThe white solid (1.0 g) was dried

Quellen und Nachweise

ORD-Eintrag
ord-b526b37c7ff642cfaae9c95924f7015f
Quelldatensatz
uspto-grants-1998_11
Patentnummer
US05834482

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