o-Aminophenethyl alcohol → Indoline

HRID 477173

Reaktionsgleichung

Reaktionsgleichung von HRID 477173
[Si]([O-])([O-])([O-])[O-].[Al+3].[Si]([O-])([O-])([O-])[O-].[Si]([O-])([O-])([O-])[O-].[Al+3].[Al+3].[Al+3].[NH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[CH2:27][CH2:28]O>>[NH:20]1[C:21]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH2:27][CH2:28]1

Komponenten

3

Edukt 2

HCID 79282o-Aminophenethyl alcoholHCID 21981400Tetraaluminum;trisilicate

Produkt 1

HCID 10328Indoline

Reaktionsbedingungen

Temperatur
220 °C

Versuchsvorschrift

In a stainless steel reactor equipped with distillation column, 5.0 g of a commercially available amorphous aluminium silicate (KETJEN® C-25-W) consisting of 14.7% by weight of AL2O3 and 82.5% by weight of SiO2, and having a BET inner surface area of 547 m2 /g and a pore volume of 0.61 cm3 /g, are suspended in 130 g (117 ml) of 2-(2'-aminohenyl)ethanol using a magnetic stirrer. The suspension is heated to 220° C. Then, at a constant reaction temperature of 220° C. and under an initial pressure of 0.5 bar, the resultant indoline/water mixture is distilled off through the packed column at an average rate of 60 g of indoline per hour. During this distillation, the volume in the reactor is kept constant with a level probe by the continuous addition of fresh 2-(2'-aminophenyl)ethanol. The reduction in the distillation rate caused by the formation of high-boiling by-products is compensated for by gradually lowering the pressure for maintaining the distillation rate over the duration of the experiment form 0.5 to 0.07 bar. After a reaction time of 150 hours, the addition of 2-(2'-aminophenyl)ethanol is discontinued and the indoline present in the reactor is distilled off under reduced pressure affording 9.0 kg of indoline in 99.5% purity as distillate. 55 g of high-boiling by-products of unknown constitution are obtained as distillation residue. The yield of indoline is 98-99% of theory.

Aufarbeitung

  1. distillationThen, at a constant reaction temperature of 220° C. and under an initial pressure of 0.5 bar, the resultant indoline/water mixture is distilled off through the packed column at an average rate of 60 g of indoline per hour
  2. distillationDuring this distillation
  3. additionthe volume in the reactor is kept constant with a level probe by the continuous addition of fresh 2-(2'-aminophenyl)ethanol
  4. temperaturefor maintaining the distillation rate over the duration of the experiment
  5. customform 0.5 to 0.07 bar
  6. distillationthe indoline present in the reactor is distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-30758fb0df944a529648f673ce2baad1
Quelldatensatz
uspto-grants-1989_12
Patentnummer
US04886887

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