2 w that a catalyst fragment CO (CO)~-has served as an oxymethylating agent equivalent (1, R= silyl). The catalytic reaction proceeds under mild reaction conditions (25 OC and 1 atm) and exhibits high regio-and stereoselectivities in many cases studied. The conversion of 2 to 3 (eq 1) was performed as follows. To a IO-mL flask containing Co2 (CO)*(0.1 mmol) was added HSiEtzMe (7.5 mmol) via syringe at 25 OC under the atmosphere of CO. In about 5 ...