in further solvent(s) soln. NaBH4 in triglyme was added slowly for 3 h at room temp. to BF3-tert-butyl methyl etherate; B2H6 was absorbed with THF, NaBF4 was filtered off, solvent was removedby distillation to obtaine more NaBF4;
in further solvent(s) soln. NaBH4 in triglyme was added slowly for 1 h at room temp. to BF3-triglymate; B2H6 was absorbed with THF, NaBF4 was filtered off, solvent was removedby distillation to obtaine more NaBF4;
in dichloromethane; water H2O and CH2Cl2 were purged with N2 for 5 min. To this stirred soln. was added (C5(CH3)5Ir(BT))(BF4)2 and then NaBH4. After 5 min the layers were separated, and the water layer was extracted with CH2Cl2.; After 5 min the layers were separated, and the water layer was extd. with CH2Cl2. The combined CH2Cl2 extracts were dried over Na2SO4 and filtered. Product was pptd. by addn. of ether. elem. anal.; ratio of isomers: 61:25:8:6;
in dichloromethane; water H2O and CH2Cl2 were purged with N2 for 5 min. To this stirred soln. was added (C5(CH3)5Ir(2-MeBT))(BF4)2 and then NaBH4.; After 5 min the layers were sepd., and the water layer was extd. with CH2Cl2. The combined CH2Cl2 extracts were dried over Na2SO4 and filtered. Product was pptd. by addn. of Et2O. elem. anal.; ratio of isomers: 60:23:9:8;
in dichloromethane; water To a stirred soln. of Cp(CH3)5Ir(3-MeBT)(BF4)2 in H2O and CH2Cl2 was added NaBH4 (under N2).; After 3 min the layers were sepd., and the water layer was extd. with CH2Cl2. The combined CH2Cl2 extracts were dried over Na2SO4 and filtered. Product was pptd. by addn. of Et2O. elem. anal.; ratio of isomers: 58:27:8:7;
