Sodium borohydride → HCID 90412642, compound

Participants

Reaction Conditions

Reaction Steps

A solution of compound 6 (from Example 6b) was added to the reactor and cooled to 0° C. 2.2 kg MeOH was added followed by addition of CeCl3.7H2O (355 g) and the mixture stirred for 1 h to result homogeneous solution. NaBH4 (8.8 g) was added in portions at 0° C., stirred for 30 min, IPC showed the reaction started and additional NaBH4 (30 g) was added in portions with stirring for 1 h at 0° C. IPC showed complete consumption of compound 6. Saturated NH4Cl (0.27 kg) was added followed by celite (266 g) and the mixture stirred for 30 min after which it was filtered, washed with water (12 L×3), and dried over Na2SO4 to give compound 7 in MTBE solution (5.5 kg), which was concentrated (below 40° C.) to furnish a residue. DMF (3 kg) was added and the solution was used directly in the next step.

Provenance & Evidence