Hydrochloric Acid → HCID 123358145, Verbindung

HRID 1470527Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1470527
[CH3:1][C:2]([C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([O:12][CH3:13])[CH:5]=1)=[O:3].[C:14]1([NH:20][C:21]2[N:28]=[CH:27][CH:26]=[CH:25][C:22]=2[CH:23]=O)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.Cl>CO>[CH3:13][O:12][C:6]1[CH:5]=[C:4]([C:2](=[O:3])[CH:1]=[CH:23][C:22]2[C:21]([NH:20][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)=[N:28][CH:27]=[CH:26][CH:25]=2)[CH:9]=[CH:8][C:7]=1[O:10][CH3:11]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 143283,4-Dimethoxyphenyl methyl ketoneHCID 13983610HCID 13983610, Verbindung

Produkt 1

HCID 123358145HCID 123358145, VerbindungAusbeute 90,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 3,4-dimethoxyacetophenone (182 mg, 1.01 mmol) in methanol (5 mL) was added 2N Ba(OH)2solution (2 mL) and stirred for 5 minutes. Then added 2-(phenylamino)nicotinaldehyde (200 mg, 1.01 mmol) and the reaction mixture was stirred at a temperature of 30° C. for 6h and the reaction was monitored by TLC. After 8h the reaction mixture was acidified with 2N HCl. The resulting precipitate was filtered, washed thoroughly with water and dried over anhydrous CaCl2. The precipitate was recrystallized using ethanol to obtain pure (6b) (328.5 mg, 90% yield).

Aufarbeitung

  1. filtrationThe resulting precipitate was filtered
  2. washwashed thoroughly with water
  3. dry with materialdried over anhydrous CaCl2
  4. customThe precipitate was recrystallized

Quellen und Nachweise

ORD-Eintrag
ord-70a929a6965e4ebb910d2507672aaa97
Quelldatensatz
uspto-grants-2015_04
Patentnummer
US09006451B1

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