1,2,3,6,-tetrahydro-N-(2-hydroxyethyl)phthalimide → HCID 10896667, Verbindung

HRID 1422265Notizen

Reaktionsgleichung

[OH:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]2[CH2:10][CH:11]=[CH:12][CH2:13][CH:6]2[C:5]1=[O:14].[C:15]([O:30]CC(C)C)(=O)[CH:16]1[CH2:28][CH:27]=[CH:26][CH2:25][CH:17]1[C:18]([O:20][CH2:21][CH:22](C)C)=[O:19]>[O-]CCCC.[O-]CCCC.[O-]CCCC.[O-]CCCC.[Ti+4].O>[C:18]([O:20][CH2:21][CH2:22][N:4]1[C:5](=[O:14])[CH:6]2[CH2:13][CH:12]=[CH:11][CH2:10][CH:7]2[C:8]1=[O:9])(=[O:19])[CH:17]1[CH2:25][CH:26]=[CH:27][CH2:28][CH:16]1[C:15]([O:1][CH2:2][CH2:3][N:4]1[C:8](=[O:9])[CH:7]2[CH2:10][CH:11]=[CH:12][CH2:13][CH:6]2[C:5]1=[O:14])=[O:30]

Komponenten

Reaktionsbedingungen

Temperatur: 230 °C

Versuchsvorschrift

N-(2-Hydroxyethyl)-1,2,3,6-tetrahydrophthalimide (195.2 g, 1 mol) was dissolved in diisobutyl 1,2,3,6-tetrahydrophthalate (141.2 g, 0.5 mol). The mixture was kept at 150° C. under vacuum to eliminate any traces of water. Titanium tetrabutoxide (1.7 g) was added under atmospheric pressure and the transesterification reaction was carried out distilling off the isobutyl alcohol formed. As the reaction proceeded the temperature was increased stepwise to 230° C. and the pressure was lowered to 20 Torr (26.7 mbar). After ca. 24 h, 265 g of brown crude bis[2-(1,2,3,6-tetrahydrophthalimido)ethyl] 1,2,3,6-tetrahydrophthalate were obtained.

Aufarbeitung

customwas kept at 150° C. under vacuum
customthe transesterification reaction
distillationwas carried out distilling off the isobutyl alcohol
customformed

Quellen und Nachweise

ORD-Eintrag: ord-2ed3f2956efc461882cb3ca99b5c14d4
Quelldatensatz: uspto-grants-2000_06
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US06080872

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