4-(Dimethylamino)benzoic acid → HCID 12810404, Verbindung

HRID 258824

Reaktionsgleichung

Reaktionsgleichung von HRID 258824
[C:1]1([CH:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:20][N:21]([CH3:31])[C:22]1[CH:30]=[CH:29][C:25]([C:26](O)=[O:27])=[CH:24][CH:23]=1>ClCCl>[CH3:20][N:21]([CH3:31])[C:22]1[CH:30]=[CH:29][C:25]([C:26]([N:11]2[CH2:10][CH2:9][CH:8]([CH:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:13][CH2:12]2)=[O:27])=[CH:24][CH:23]=1

Komponenten

4

Edukt 2

HCID 120924-(Dimethylamino)benzoic acid2×HCID 882784-Benzhydrylpiperidine

Produkt 1

HCID 12810404HCID 12810404, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

To a solution of 150 parts of 4-(diphenylmethyl)piperidine and 99 parts of 4-(dimethylamino)benzoic acid in 4000 parts of dichloromethane is added a solution of 123 parts of N,N1 -methanetetraylbiscyclohexanamine in 1330 parts of dichloromethane. The resultant mixture is stirred for 6 hours, whereupon a further 25 parts of 4-(dimethylamino)benzoic acid and 30 parts of N,N1 -methanetetraylbiscyclohexanamine is introduced and stirring continued thereafter for 24 hours. The reaction mixture is then filtered, and the filtrate is stripped of solvent by vacuum distillation. The residue is taken up in ether; and the ether solution is consecutively washed with 5% hydrochloric acid, water, and 5% ammonium hydroxide, then dried over anhydrous potassium carbonate and finally stripped of solvent by vacuum distillation. The residue is recrystallized from a mixture of benzene and hexane to give 1-[4-(dimethylamino)benzoyl]-4-(diphenylmethyl)piperidine melting at 177°-179°.

Aufarbeitung

  1. additionis introduced
  2. filtrationThe reaction mixture is then filtered
  3. distillationthe filtrate is stripped of solvent by vacuum distillation
  4. washand the ether solution is consecutively washed with 5% hydrochloric acid, water, and 5% ammonium hydroxide
  5. dry with materialdried over anhydrous potassium carbonate
  6. distillationfinally stripped of solvent by vacuum distillation
  7. customThe residue is recrystallized from a mixture of benzene and hexane

Quellen und Nachweise

ORD-Eintrag
ord-dadc7376b1c94fbcb7582c200eed6207
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04035372

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