Bis(4-hydroxyphenyl)methane → HCID 20510578, Verbindung

HRID 1758203Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1758203
[CH2:1]([N:5]1[C:9](=[O:10])[C:8]2([CH2:15][C:14]([CH3:17])([CH3:16])[N:13]([CH2:18][CH:19]3[O:21][CH2:20]3)[C:12]([CH3:23])([CH3:22])[CH2:11]2)[NH:7][C:6]1=[O:24])[CH2:2][CH2:3][CH3:4].[OH:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][C:33]2[CH:38]=[CH:37][C:36]([OH:39])=[CH:35][CH:34]=2)=[CH:28][CH:27]=1.[H-].[Na+]>C(O)CC(C)C>[CH2:1]([N:5]1[C:9](=[O:10])[C:8]2([CH2:11][C:12]([CH3:22])([CH3:23])[N:13]([CH2:18][CH:19]([OH:21])[CH2:20][O:25][C:26]3[CH:27]=[CH:28][C:29]([CH2:32][C:33]4[CH:38]=[CH:37][C:36]([O:39][CH2:20][CH:19]([OH:21])[CH2:18][N:13]5[C:14]([CH3:17])([CH3:16])[CH2:15][C:8]6([NH:7][C:6](=[O:24])[N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:9]6=[O:10])[CH2:11][C:12]5([CH3:22])[CH3:23])=[CH:35][CH:34]=4)=[CH:30][CH:31]=3)[C:14]([CH3:17])([CH3:16])[CH2:15]2)[NH:7][C:6]1=[O:24])[CH2:2][CH2:3][CH3:4]

Komponenten

5

Versuchsvorschrift

A mixture of 4.0 g of 3-butyl-8-(2,3-epoxypropyl)-7,7,9,9-tetramethyl-1,3,8-triazaspiro[4.5]decane-2,4-dione and 1.0 g of bis(p-hydroxyphenyl)methane in 5 ml of isopentyl alcohol with a catalytic amount of sodium hydride was refluxed for 10 hours. After completion of the reaction, the residue obtained by evaporating the solvent under reduced pressure from the reaction mixture was purified by column chromatography through silica gel eluted with a 1:1 by volume mixture of benzene and ethyl acetate, giving the desired Compound No. 351 in the form of white crystals melting at 202°-204° C.

Aufarbeitung

  1. temperaturewas refluxed for 10 hours
  2. customAfter completion of the reaction
  3. customthe residue obtained
  4. customby evaporating the solvent under reduced pressure from the reaction mixture
  5. customwas purified by column chromatography through silica gel
  6. washeluted with a 1:1 by volume mixture of benzene and ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-ede89440b52340ad8bbc0763d430f07c
Quelldatensatz
uspto-grants-1983_02
Patentnummer
US04371644

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