Formic Acid → HCID 136034483, compound

Participants

Reaction Conditions

Reaction Steps

To a stirred solution of (XIII) (3.1 Kg) in ethanol (52 L), was charged a slurry of 10% Pd/C (300 g in 750 ml water) under nitrogen atmosphere. Formic acid (1.16 L) was added followed by addition of solution of ammonium formate (1.452 Kg) in DM water (755 ml). The reaction mixture was heated at 50° C. for 6 hr. The reaction mixture was cooled to room temperature and filtered. DM Water (31 L) was added to the filtrate, stirred and extracted with toluene (62 L). The organic layer was separated and washed with of (1:1) water: ethanol mixture (31 L). The organic layer was dried on sodium sulfate and evaporated up to 80%. The residual liquid was cooled to 0-5° C., filtered and dried at 50° C. for 1 hr to give the title product (XIV) (1.254 Kg). If required, the product was leached with methanol to obtain required purity.

Provenance & Evidence