[CH3:1][C@H:2]1[CH2:7][C@@H:6]([OH:8])[C@H:5]([C:9]([CH3:11])=[CH2:10])[CH2:4][CH2:3]1.[C:12]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C]=O.[H][H]>[Cr].[Co].O1CCOCC1>[CH3:10][CH:9]1[CH:5]2[CH2:4][CH2:3][CH:2]([CH3:1])[CH2:7][CH:6]2[O:8][CH:12]=[CH:11]1A 100 ml Hastelloy C autoclave was charged with 15 g of isopulegol, 0.09 g of chlorotristriphenylphosphinerhodium, 0.05 g of triphenylphosphine and 30 ml of dioxane. The autoclave was then charged with equal volumes of carbon monoxide and hydrogen which pressurized the autoclave to 100 kg/cm2. The reaction was carried out at a temperature of 140° C. and at a pressure of 90 to 120 kg/cm2 for a period of 5 hours. After cooling, the pressure was reduced to atmospheric, and the reaction mixture was recovered from the autoclave and distilled for purification which yielded 15.6 g of 4a,5,6,7,8,8a-hexahydro-4,7-dimethyl-4H-1-benzopyran having a boiling point of from 64° to 66° C. at 0.5 mmHg. The IR and NMR spectra of the product had the following absorption characteristics:
불러오는 중…
