Benzene → HCID 19973343, compound

A 5-L pressure reaction vessel was charged with a solution comprising 83.3 mg of Rh(CO)2 (CH3COCHCOCHS3), 20.87 g of tris(2,6-di-t-butylphenyl) phosphite and 500 mL of benzene, and the vessel was pressurized to 90 atm with a mixed gas of carbon monoxide/hydrogen (1/1). After the temperature had been elevated to 100° C., 2.05 kg of 2,6-dimethyl-1,7-octadiene was added over a period of 5 hours, during which the pressure was maintained at 90 atm. After completion of the feed, the reaction was continued for a further 5 hours at the same temperature and pressure. The reaction vessel was cooled and then the gas therein was purged. The reaction mixture was taken out and then benzene was distilled off under vacuum. The residue was subjected to simple distillation to remove the catalytic components. The resulting distillate was rectified to give 3,7-dimethyldecanedial as an almost colorless liquid having a boiling point of 99° to 100° C. at 0.85 mmHg. The yield was 41% (1.20 kg).

1. additionwas charged with a solution
2. customhad been elevated to 100° C.
3. temperaturewas maintained at 90 atm
4. temperatureThe reaction vessel was cooled
5. customthe gas therein was purged
6. distillationbenzene was distilled off under vacuum
7. distillationThe residue was subjected to simple distillation
8. customto remove the catalytic components

ORD record

ord-0eba06100b44493c80bb831b40971cca

Source dataset

uspto-grants-1997_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05606005