O-Xylene → HCID 86737387, Verbindung

HRID 1732726

Reaktionsgleichung

Reaktionsgleichung von HRID 1732726
[CH2:1]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:2]([C:12]([O:14][CH2:15][CH3:16])=[O:13])([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6].[CH2:22]([N:29]1[C:34]([CH3:36])([CH3:35])CC(O)[CH2:31][C:30]1([CH3:39])[CH3:38])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.[C:40]1([CH3:47])[C:41](C)=[CH:42][CH:43]=[CH:44][CH:45]=1.[Li]N>C(O)C>[CH2:22]([N:29]1[C:30]([CH3:38])([CH3:39])[CH2:31][CH:20]([O:19][C:17]([CH2:1][C:2]([C:12]([O:14][CH:15]2[CH2:31][C:30]([CH3:39])([CH3:38])[N:29]([CH2:47][C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)[C:34]([CH3:36])([CH3:35])[CH2:16]2)=[O:13])([C:7]([O:9][CH:10]2[CH2:39][C:30]([CH3:31])([CH3:38])[N:29]([CH2:22][C:23]3[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:34]([CH3:35])([CH3:36])[CH2:11]2)=[O:8])[CH2:3][CH2:4][CH2:5][CH3:6])=[O:18])[CH2:21][C:34]1([CH3:35])[CH3:36])[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

Komponenten

6

Edukt 4

HCID 7237O-XyleneHCID 1036024-Piperidinol, 2,2,6,6-tetramethyl-1-(phenylmethyl)-HCID 122968851,2,2-Hexanetricarboxylic acid, triethyl esterHCID 178506930HCID 178506930, Verbindung

Produkt 1

HCID 86737387HCID 86737387, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

30.2 g (0.1 mol) of triethyl hexane-1,2,2-tricarboxylate, 74.2 g (0.3 mol) of 1-benzyl-2,2,6,6-tetramethyl-4-hydroxypiperidine and 50 ml of xylene are warmed to 130° and mixed with 0.8 g of LiNH2. The ethanol formed is distilled off continuously. The solution is kept at the above temperature for 3 hours, so that it can then be kept at 150° for a further 2 hours. After cooling, the residue is taken up in toluene, a little glacial acetic acid is added to the solution and the latter is washed with H2O. After drying over Na2SO4, the solvent is distilled off in vacuo. Tris-(1-benzyl-2,2,6,6-tetramethyl-4-piperidinyl)hexane-1,2,2-tricarboxylate is obtained as a powdery residue. (Compound No. 1).

Aufarbeitung

  1. distillationis distilled off continuously
  2. waitcan then be kept at 150° for a further 2 hours
  3. temperatureAfter cooling
  4. additiona little glacial acetic acid is added to the solution
  5. washthe latter is washed with H2O
  6. dry with materialAfter drying over Na2SO4
  7. distillationthe solvent is distilled off in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-f49222781930484c9ba96ee7d95aca35
Quelldatensatz
uspto-grants-1980_12
Patentnummer
US04238613

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