Water → HCID 86748138, compound

Temperature

50 °C

To a 1000 ml flask thoroughly purged with nitrogen, equipped with a stirrer and a reflux condenser, 100 ml of toluene which had been dehydrated and deoxygenated was introduced. Subsequently, 0.72 g (10 mmol) of trimethylaluminium and 1.96 g (10 mmol) of triisobutylaluminium were diluted in 50 ml of toluene in one of two dropping funnels, and toluene containing saturated water was introduced to the other funnel. The mixed aluminium solution and the toluene containing saturated water were fed to the flask at 30° C. over 3 hours in such a manner that an equimolar amount of the A1 and the H2O were fed at the same time. After the feeding was completed, the mixture was heated to 50° C., and a reaction was carried out for 2 hours. After the reaction was completed, the solvent was distilled off under reduced pressure, thereby giving 1.9 g of methylisobutylalumoxane as a white solid. The white solid thus obtained was dissolved in toluene, and the solution was subjected to a measurement by 27A1-NMR. As a result, a spectrum having a chemical shift at 174 ppm with a half band width of 5844 Hz was obtained.

1. customTo a 1000 ml flask thoroughly purged with nitrogen
2. customequipped with a stirrer and a reflux condenser
3. customdeoxygenated
4. additionwas introduced
5. additionwas introduced to the other funnel
6. distillationthe solvent was distilled off under reduced pressure

ORD record

ord-78fa224cb76a4ad09f6f843e165bdf72

Source dataset

uspto-grants-1994_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05346925