Triethylamine → 3-chloro-N,N-dimethyl-4-methylamino-benzamide

HRID 2079001Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2079001
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[NH:11][CH3:12])[C:5](O)=[O:6].C(C1NC=CN=1)([C:15]1[NH:16][CH:17]=CN=1)=O.C(N(CC)CC)C>C(OCC)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[NH:11][CH3:12])[C:5]([N:16]([CH3:17])[CH3:15])=[O:6]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 230850783-Chloro-4-(methylamino)benzoic acid

Produkt 1

HCID 668685293-chloro-N,N-dimethyl-4-methylamino-benzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To 3-chloro-4-methylamino-benzoic acid (387 mg) in dry N. N-dimethylformamide (10 mL) was added carbonyl diimidazole (440 mg). After one hour, dimethylamine. HCl (221 mg) and triethylamine (0.38 mL) were added. The reaction mixture was stirred overnight, then diluted with ethyl acetate, washed with brine, dried (MgSO4) and the solvent removed in vacuo. Purification using flash chromatography yielded 3-chloro-N,N-dimethyl-4-methylamino-benzamide.

Aufarbeitung

  1. washwashed with brine
  2. dry with materialdried (MgSO4)
  3. customthe solvent removed in vacuo
  4. customPurification

Quellen und Nachweise

ORD-Eintrag
ord-41dccc01b8744ba4bf3dfd237f785fd4
Quelldatensatz
uspto-grants-2011_04
Patentnummer
US07928248B2

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