反应详情

温度

120 °C

250 mg of tert-butyl trans-[4-(4-trifluoromethanesulfonyloxyphenyl)cyclohexyloxy]-acetate are placed in 1.5 mL of dioxane in a microwave tube. 83 mg of hexacarbonylmolybdenum (0.32 mmol, 0.5 eq.), 14 mg of palladium diacetate (0.06 mmol, 0.1 eq.), 35 mg of DPPF (0.06 mmol, 0.1 eq.), 154 mg of DMAP (1.26 mmol, 2 eq.), 0.25 mL of DIEA (1.45 mmol, 2.3 eq.) and 0.23 mL of water are successively added. The tube is sealed and heated by microwave at 120° C. for 30 minutes. The reaction medium is diluted with dichloromethane and washed three times with saturated aqueous sodium carbonate solution. The reaction medium is diluted with diethyl ether and washed with aqueous 5N HCl solution. The organic phases are combined and evaporated to give 270 mg of trans-4-(4-tert-butoxycarbonylmethoxycyclohexyl)benzoic acid, which is used without further purification in the following step.

1. customThe tube is sealed
2. washwashed three times with saturated aqueous sodium carbonate solution
3. additionThe reaction medium is diluted with diethyl ether
4. washwashed with aqueous 5N HCl solution
5. customevaporated