Yield:-

Reaction Conditions:

with ammonia;hydrogen;Raney Nickel (Ra-Ni) in methanol;water; under 2327.23 Torr; for 15.5 h;Parr apparatus;

Steps:

3

To a solution of the previous compound (363 mg ; 1.20 mmol) in 2.0 M ammonia in methanol (5 ml) was added Raney Nickel (approx. 0.5 ml of 50% aqueous slurry) and the mixture agitated under an atmosphere of hydrogen (45 psi) on a Parr apparatus for 15.5 hours. The mixture was filtered through a catalyst filter and the catalyst washed extensively with methanol (5 x 25 ml). The solvent was evaporated to give the desired compound as a green oil which was used directly in the next step (351 mg). m/e = 306.

References:

WO2006/67529,2006,A1 Location in patent:Page/Page column 40