反应详情

To a solution of 66 (299.4 mg, 0.72 mmol) in CHCl3 (5 mL) was added a 10% (v) solution of Br2 in chloroform. The reaction was stopped when starting material was consumed, monitored by HPLC. Bromine was quenched with a saturated Na2SO3 solution and product extracted with DCM (2×10 mL). Organics were washed with water (2×10 mL) and brine (1×10 mL) and dried over Na2SO4. Purified by flash column eluting 10% methanol in ethyl acetate. Evaporation of solvent gave 223.6 mg (63%) of 67 as a yellow solid. LCMS: m/z for C20H28BrN6O2P++H observed 495.2 and 497.2 at 1.98 minutes of a 3.5 minute run, eluting 5-95% CH3CN in H2O.

1. customwas consumed
2. customBromine was quenched with a saturated Na2SO3 solution and product
3. extractionextracted with DCM (2×10 mL)
4. washOrganics were washed with water (2×10 mL) and brine (1×10 mL)
5. dry with materialdried over Na2SO4
6. customPurified by flash column
7. washeluting 10% methanol in ethyl acetate
8. customEvaporation of solvent