o-Aminophenethyl alcohol → Indoline

関与物質

反応条件

反応手順

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.

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