Hydrochloric Acid → (R)-4-methyl-6-(3-methyl-azetidin-3-ylamino)-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one

Participants

Reaction Steps

A suspension of (R)-6-(1-benzhydryl-3-methyl-azetidin-3-ylamino)-4-methyl-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (Example #148, Step E, 20 g, 42.8 mmol) and PdOH2/C(10%, 10 g, 71.2 mmol) in MeOH (400 mL) and HCl (2 mL) was stirred at 50° C. under H2 (50 psi) for 48 h. The reaction mixture was cooled to ambient temperature and filtered, washed with hot MeOH (3×100 mL). The combined filtrate was concentrated in vacuo to give (R)-4-methyl-6-(3-methyl-azetidin-3-ylamino)-2,10-dihydro-9-oxa-1,2,4a-triaza-phenanthren-3-one (18 g, 99%), which was used directly. LC/MS (Table 1, Method 25) Rt=0.525 min.; MS m/z: 302 [M+H]+.

Provenance & Evidence