Water → HCID 51033188, compound

Participants

Reaction Steps

A solution was prepared with 301.5 mg (1S,6R)-6-(3,4-dichlorophenyl)-1-[(methyloxy)methyl]-3-azabicyclo[4.1.0]heptane (E2a, oil) and 0.2 mL aqueous isopropylalcohol 5% w/w water (aq. IPA). To this solution 209.6 microL of phosphoric acid (5M in water) was added with stirring. A further 0.1 mL of solvent was added while stirring yielding a slurry. 0.3 mL and then 0.1 mL of solvent were added to give a mobile slurry. (Total aq. IPA added 0.7 mL). The resulting slurry was temperature cycled between 0 and 40° C. for 24 hours. The sample was then filtered and the solid title compound obtained dried under vacuum at 70° C. for 24 hours.

Provenance & Evidence