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With hydrogen; In propan-1-ol; at 240℃; under 207625 Torr; for 3.0h;Autoclave;
10 g of copper catalyst (E406 from BASF) was packed in a stainless steel basket, which was then installed in a 100 ml autoclave (HEL). Then, the catalyst was treated in the autoclave with 1500 psig hydrogen at 200°C for 2 hours. After the autoclave was cooled to 80 °C and the hydrogen pressure was reduced to 100 psig, 60 g of 10percent dimethyl bicyclo[2.2.2]octane-1 ,4-dicarboxylate in n-propanol was added to the autoclave with a blowcase; thus, the reaction started. After three hours at 240 °C and 4000 psig hydrogen, the reaction was stopped, and the product was analyzed with a GC. Dimethyl bicyclo[2.2.2]octane-1 ,4-dicarboxylate conversion was 100percent and bicyclo[2.2.2]octane-1 ,4-diyldimethanol selectivity was 100percent.
With [2-(di-tert-butylphosphinomethyl)-6-(diethylaminomethyl)pyridine]carbonylchlorohydridoruthenium (ll); hydrogen; potassium hydroxide; In para-xylene; at 140℃; under 39547.2 - 52476.2 Torr; for 8.0h;Autoclave;
At atmospheric conditions, 0.1 g of the Milstein catalyst precursor [2-(Di-tert- butylphosphinomethyl)-6- (0259) (diethylaminomethyl)pyridine]carbonylchlorohydridoruthenium(ll), 30 mg of potassium hydroxide, 2.5g of dimethyl bicyclo[2.2.2]octane-1 ,4-dicarboxylate and 50 imL of p- xylene were added to a 100 imL autoclave reactor. The reactor was then purged three times by pressurizing with nitrogen to 200 psig, then venting the pressure to atmospheric each time. The reactor was then purged three times by pressurizing with hydrogen to approximately 300 psig, then venting the pressure to atmospheric each time. Agitation at 800 rpm was then commenced, and hydrogen was then added to bring the pressure to 750 psig. The temperature was then increased to 140 °C while allowing pressure to rise. After the temperature reaches 140 °C, the hydrogen pressure was increased to 1000 psig. These conditions (140 °C and 1000 psig) were held for 8 hours of reaction. After 8 hours of reaction, the agitation was stopped and the heat turned off to let the autoclave start cooling. After cooling to room temperature, pressure was released, and the contents were purged with nitrogen gas and vented. The solution was finally discharged from the autoclave and analyzed by GC-MS and 1H NMR. The conversion of dimethyl bicyclo[2.2.2]octane-1 ,4-dicarboxylate is 94percent; the selectivity of bicyclo[2.2.2]octane-1 ,4-diyldimethanol is 93percent; and the selectivity of methyl 4-(hydroxymethyl)bicyclo[2.2.2]octane-1 -carboxylate is 7percent.
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